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Epoxy Composites
Epoxy Composites
Fabrication, Characterization and Applications
Edited by
Jyotishkumar Parameswaranpillai
Harikrishnan Pulikkalparambil
Sanjay M. Rangappa
Suchart Siengchin
Editors All books published by Wiley-VCH
are carefully produced. Nevertheless,
Dr. Jyotishkumar Parameswaranpillai authors, editors, and publisher do not
King Mongkut’s University of warrant the information contained in
Technology North Bangkok (KMUTNB) these books, including this book, to
Department of Materials and Production be free of errors. Readers are advised
Engineering to keep in mind that statements, data,
1518 Pracharaj 1 illustrations, procedural details or other
Wongsawang Road, Bangsue items may inadvertently be inaccurate.
10800 Bangkok
Thailand Library of Congress Card No.:
applied for
Mr. Harikrishnan Pulikkalparambil
King Mongkut’s University of British Library Cataloguing-in-Publication
Technology North Bangkok (KMUTNB) Data
Department of Materials and Production A catalogue record for this book is
Engineering available from the British Library.
1518 Pracharaj 1
Wongsawang Road, Bangsue Bibliographic information published by
10800 Bangkok the Deutsche Nationalbibliothek
Thailand The Deutsche Nationalbibliothek lists
this publication in the Deutsche
Dr. Sanjay M. Rangappa Nationalbibliografie; detailed
King Mongkut’s University of bibliographic data are available on the
Technology North Bangkok Internet at <http://dnb.d-nb.de>.
Department of Materials and Production
Engineering © 2021 WILEY-VCH GmbH, Boschstr.
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part of this book may be reproduced in
Prof. Suchart Siengchin any form – by photoprinting,
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Cover Image: © Igor Krutov/Alamy Stock Print ISBN: 978-3-527-34678-3

Photo ePDF ISBN: 978-3-527-82406-9
ePub ISBN: 978-3-527-82407-6
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v
Contents
1 Introduction to Epoxy Composites 1

Harikrishnan Pulikkalparambil, Sanjay Mavinkere Rangappa, Suchart
Siengchin, and Jyotishkumar Parameswaranpillai
1.1 Introduction 1
1.2 Manufacturing Methods for Fabrication of Epoxy Composites 2
1.3 Experimental Techniques for the Characterization of Epoxy
Composites 3
1.4 Properties of Epoxy Composites 6
1.4.1 Mechanical Properties 6
1.4.2 Dielectric Properties 9
1.4.3 Water/Moisture Absorption 9
1.4.4 Morphology 11
1.5 Conclusion 13
References 13
2 Synthesis and Manufacturing of Epoxy Composites 23

Turup P. Mohan and K. Kanny
2.1 Introduction 23
2.2 History of Epoxy Resin 23
2.3 Types of Epoxy Resins 24
2.3.1 Bisphenol-A Epoxy Resin 24
2.3.2 Bisphenol-F Epoxy Resin 24
2.3.3 Phenol Novolac Epoxy Resin 25
2.3.4 Cycloaliphatic Epoxy Resin 26
2.3.5 Epoxy Resin Diluents 26
2.3.6 Glycidylamine Epoxy Resin 27
2.4 Curing 27
2.4.1 Curing Agents 27
2.4.1.1 Polyaddition Reactions (Active Hydrogen Compounds) 28
2.4.1.2 Polyamide and Polyamine 28
2.4.1.3 Secondary and Tertiary Amines 30
2.4.2 Anionic and Cationic Initiators 31
vi Contents
2.4.2.1 Imidazole (Anionic Polymerizing) 31

2.4.2.2 Polymercaptan 31
2.4.2.3 Anhydrides 32
2.4.2.4 Canhydrides 32
2.4.2.5 Alicyclic Anhydrides 32
2.4.2.6 Aliphatic Anhydrides 32
2.4.3 Latent Curing Agents 32
2.4.3.1 Light-Curing and Ultraviolet-Curing Agents 33
2.4.3.2 Boron Trifluoride–Amine Complex 33
2.4.3.3 Dicyandiamide 33
2.4.3.4 Organic-Acid Hydrazide 33
2.4.4 Curing Conditions 34
2.4.4.1 Bisphenol-A Epoxy Resin 34
2.4.4.2 Bisphenol-F Epoxy Resin 34
2.4.4.3 Phenol Novolac Epoxy Resin 34
2.4.4.4 Cycloaliphatic Epoxy Resin 34
2.4.4.5 Glycidylamine Epoxy Resin 34
2.5 Reaction Mechanisms 34
2.5.1 Bisphenol-A Epoxy Resin 34
2.5.2 Bisphenol-F Epoxy Resin 35
2.5.5 Epoxy Resin Diluents 36
2.6 Safety and Environmental Factors of Epoxy Resins 36
2.6.1 Bisphenol-A Epoxy Resin, Bisphenol-F Epoxy Resin, Glycidylamine
Epoxy Resin, Epoxy Resin Diluents 36
2.6.1.1 Health Risks 36
2.6.1.2 Environmental Issues 36
2.7 Manufacturing of Epoxy Composites 37
2.7.1 Open Molding 37
2.7.1.1 Hand Lay-Up 38
2.7.1.2 Spray-Up 39
2.7.1.3 Filament Winding 40
2.7.2 Closed Molding 41
2.7.2.1 Reinforced Reaction Injection Molding (RRIM) 41
2.7.2.2 Vacuum-Assisted Resin Transfer Molding Process (VARTM) 43
2.7.2.3 Light Resin Transfer Molding (LRTM) 44
2.7.2.4 Vacuum Infusion Process (VIP) 45
2.7.2.5 Pultrusion Process 46
Contents vii
2.7.2.6 Vacuum Bag Molding (Wet Bagging) 47

2.7.2.7 Centrifugal Casting 48
2.7.3 Natural Fiber Reinforced Epoxy Composites 49
2.7.3.1 Manufacturing of Natural Fiber Reinforced Epoxy Composites 49
2.8 Preparing of Particulate Filled Epoxy Composites 51
2.8.1 Particle Reinforced Epoxy Composites 51
2.8.2 Nanoparticle-Filled Epoxy Composite 51
2.8.2.1 Method 1 52
2.8.2.2 Method 2 52
2.9 Futuristic Processing of Epoxy-Based Composites 52
2.9.1 Fast Curing Powder Adhesive Epoxy Resin 52
2.9.2 3D Printing 53
2.9.3 Adhesive Method 53
2.9.4 Ultrasonic Fabrication Method for Epoxy Resin/SbSI Nanowire
Composites 54
2.9.5 Electron-Beam (E-Beam) Curing 54
2.9.6 Automated Fiber Placement (AFP) Epoxy Resin Composite 54
2.10 Conclusion 54
References 55
3 Micro- and Nanoscale Structure Formation in Epoxy-Clay

Nanocomposites 61
Seno Jose, V. K. Smitha, Sanjay M. Rangappa, Senthilkumar Krishnasamy,
Debabrata Nandi, Suchart Siengchin, and Jyotishkumar Parameswaranpillai
3.1 Introduction 61
3.2 Micro and Nanoscale Structures of Polymer/Clay Nanocomposites 62
3.3 Evolution of Epoxy-Clay Nanocomposite Structure 65
3.4 Mechanism of Nanocomposite Formation 67
3.5 Conclusion and Future Outlook 72
References 73
4 Long Fiber-Reinforced Epoxy Composites 83

Ayesha Kausar
4.1 Introduction 83
4.2 Long Fiber Fillers 84
4.3 Long Fiber-Reinforced Epoxy Composite 84
4.3.1 Epoxy and Long Glass Fiber Composite 84
4.3.2 Epoxy and Long Carbon Fiber Composite 87
4.3.3 Epoxy and Natural Fiber Composite 90
4.4 Applications, Future Prospective, and Summary 90
References 92
5 Eco-Friendly Epoxy-Based Composites 97

Vivek Mishra and Alok Agrawal
5.1 Introduction 97
viii Contents
5.2 Physical Behavior of Natural Fiber/Filler-Reinforced Epoxy

Composites 100
5.3 Mechanical Properties of the Epoxy-Based Composites 103
5.3.1 Tensile Properties 104
5.3.2 Impact Properties 106
5.4 Thermal Behavior of Natural Fiber/Filler-Reinforced Epoxy
Composites 108
5.5 Wear Behavior of Natural Fiber/Filler-Reinforced Epoxy
Composites 115
5.5.1 Erosive Wear 115
5.5.2 Adhesive Wear 115
5.5.3 Abrasive Wear 116
5.6 Bioepoxy Composites 118
5.7 Conclusion 119
References 119
6 Processing of Epoxy Composites Based on Carbon

Nanomaterials 125
Lourdes Ramos-Galicia, Juventino López-Barroso, Julio Alejandro
Rodríguez-González, Carlos Velasco-Santos, Carlos Rubio-González,
and Ana Laura Martínez-Hernández
6.1 Introduction 125
6.2 Epoxy Nanocomposites Reinforced with 1D and 2D Carbon Materials,
Mechanical and Thermomechanical Performance 126
6.3 Tracing of Cure Reaction 136
6.3.1 1D Carbon Nanostructures Influence over the Epoxy Cure Reaction 137
6.3.2 Influence of 2D Carbon Nanostructures Over the Cure Reaction 139
6.3.3 3D Hybrid Carbon Nanostructures over Cure Reaction of Epoxy
Nanocomposites 143
6.4 Improved Mechanical Properties of Carbon Fiber Reinforced Polymers
(Epoxy) through the Incorporation of Carbon Nanostructures 146
6.4.1 CFRPs (Based Epoxy) Modified with Carbon Nanotubes 147
6.4.2 CFRPs (Based Epoxy) Modified with Graphene-Based Materials 154
6.4.3 CFRPs (Based Epoxy) Modified with Hybrids (Carbon Nanotubes and
Graphene) 158
6.5 Concluding Remarks 160
References 161
7 Thermal Stability and Flame Retardancy of Epoxy

Composites 177
Mohamedismail Fathima Rigana, Tharakan Simi Anne, Sadhasivam Balaji,
Shanmugam Chandrasekar, and Muthusamy Sarojadevi
7.2 Effects of Micro Fillers on Thermal Properties of Epoxy Resin 178
7.2.1 Epoxy/Glass Fiber Composites 178
Contents ix
7.2.1.1 Bis(4-cyanato-3,5-dimethylphenyl) Naphthyl Methane/Epoxy/Glass

Fiber Composites 178
7.2.1.2 Epoxy (DGEBA) Resin + CSE (Chlorinated Soy Oil) – Based Epoxy/Glass
Fiber Composites 179
7.2.1.3 Novolac-Type Epoxy and Isocyanate-Modified Epoxy/Glass Fiber
Composites 182
7.2.2 Epoxy/Natural Fiber Composites 182
7.2.2.1 Epoxy (DER 331)/Kenaf Fiber Composites 182
7.2.2.2 Epoxy (Ampreg 26)/Phormium tenax Composites 185
7.2.3 Epoxy/Natural Fiber Hybrid Composites 186
7.2.3.1 Epoxy (Araldite M)/Jute–Glass Fiber Hybrid Composites 186
7.2.3.2 Epoxy/Flax and Sisal–Glass Fiber Composites 186
7.2.3.3 Epoxy (DER 331)/MH (Magnesium Hydroxide)-Kenaf Fiber
Composites 187
7.3 Effect of Nanofillers on Thermal Properties of Epoxy Resin 188
7.3.1 Epoxy/Clay Nanocomposites 188
7.3.1.1 Epoxy (DGEBA)/Clay Nanocomposites 188
7.3.1.2 Epoxy (E51)/D-clay (Na+ -MMT) Nanocomposites 189
7.3.1.3 Epoxy (DGEBA)/Cloisite Na+, Cloisite 10A, Cloisite 15, Cloisite 93A
Nanocomposites 190
7.3.1.4 Organo Phosphorus Epoxy/Clay Nanocomposite 190
7.3.1.5 Epoxy (DGEBA)/DNA-Modified MMT Clay Nanocomposites 191
7.3.2 Epoxy/CNF Nanocomposites 192
7.3.2.1 Epoxy (SC-15)/Carbon Nano Fiber (PR-24) Nanocomposites 192
7.3.3 Epoxy/CNT Nanocomposites 194
7.3.3.1 CNT/Epoxy Nanocomposites 194
7.3.4 Epoxy/Cellulose Nanofiber Nanocomposites 196
7.3.4.1 Epoxy (D.E.R. 331)/Cellulose Nanofiber Nanocomposites 196
7.3.5 Epoxy/Spherical Metal Oxide Nanocomposites 196
7.3.5.1 Epoxy (Epon 862)/Coreshell Fe@FeO Nanocomposites 196
7.3.5.2 Epoxy (Epon 862)/Polyaniline-Stabilized Silica Nano Composites 199
7.3.6 Epoxy Based Hybrid Nanocomposites 201
7.3.6.1 Epoxy (DGEBA)/CNT/OMPOSS/APP Hybrid Nanocomposite 201
7.3.6.2 Acrylonitrile–Butadiene–Styrene/Brominated Epoxy–Antimony
Oxide/Organo Montmorillonite (ABS/BER-AO/OMT)
Nanocomposites 202
7.3.6.3 Epoxy/Ag@Cu–Ag@rGO Nanocomposite-Based Conductive
Adhesives 203
7.3.6.4 Epoxy/HM-SiO2 @CeO2 /NiO Nanocomposites 203
7.3.6.5 Epoxy (Araldite)/Microsilica/Nanoalumina Nanocomposites 204
7.4 Epoxy-Based Hybrid Micro and Nanocomposites 204
7.4.1 Epoxy (LY556)–Closite 25A OMMT/Glassfiber Micro Nano
Composite 204
7.4.2 Epoxy/Glass Fiber (GE) Composites, Epoxy/Glass Fiber/FGO
Nanocomposites 205
x Contents
7.4.3 Epoxy/Glass Fiber (GE) Composites and Epoxy/Glassfiber/Nano Al2 O3

Nanocomposites 205
7.4.4 Epoxy/CF/DWCNT-NH2 Micro-Nanocomposites 206
7.4.5 Epoxy/Carbon Fiber Composites, Epoxy/Carbon Nanotube
Membrane/Carbon Nanofiber (CNF) Paper Micro-Nanocomposites 207
7.5 Conclusions 211
Acknowledgments 212
References 212
8 Spectroscopy and X-ray Scattering Studies of Epoxy

Composites 217
P. Poornima Vijayan
8.2 In situ Cure Monitoring 218
8.3 Characterization of Interface in Fiber-Reinforced Epoxy
Composites 225
8.4 Determination of Residual Stress Developed During Cure 228
8.5 Stress Transmission Studies in Particulate Filled Epoxy Composite 231
8.6 Water Diffusion Studies 232
8.7 Morphological Analysis in Epoxy Composites 233
8.8 Conclusion 236
References 236
9 Water Absorption Studies in Epoxy Nanocomposites 241

Bejoy Francis
9.2 Factors Affecting Water Absorption 242
9.3 Effect of Water Absorption on Mechanical Properties 247
9.4 Effect of Water Absorption on Dynamic Mechanical Properties 251
9.5 Effect of Water Absorption on Thermomechanical Properties 253
9.6 Effect of Water Absorption on Dielectric Properties 254
9.7 Conclusion 255
References 255
10 Fracture Surface and Mechanical Properties of Epoxy

Composites 259
Mehdi Naderi and Farnaz Ebrahimi
10.2 Morphology 266
10.2.1 Dispersion and Interfacial Adhesion 266
10.2.2 Fracture Surface Morphology 273
10.3 Mechanical Properties 278
10.3.1 Stress–Strain Behavior 278
10.3.2 Fracture Toughness 281
10.3.3 Impact Properties 282
Contents xi
10.3.4 Dynamic Mechanical Properties 284

10.3.5 Lap Shear Properties 288
10.4 Conclusions and Outlooks 290
References 292
11 Dielectric and Conductivity Studies of Epoxy Composites 299

Anastasios C. Patsidis and Georgios C. Psarras
11.2 Experimental Techniques and Data Interpretation 300
11.2.1 Experimental Techniques 300
11.2.2 Dielectric and Conductivity Data Interpretation 300
11.3 Electrical Properties of Epoxy Resins 302
11.4 Epoxy/Nonconductive Reinforcing Phase Composites 306
11.4.1 Epoxy/Nonconductive Filler Micro-composites 306
11.4.2 Epoxy/Nonconductive Filler Nanocomposites 312
11.5 Epoxy/Conductive Reinforcing Phase Composites 317
11.5.1 Epoxy/Conductive Filler Micro-composites 317
11.5.2 Epoxy/Conductive Filler Nanocomposites 325
11.6 Epoxy-Based Hybrid Composites – Targeting Multifunctionality 332
11.7 Conclusions and Future Trends 343
References 343
12 Smart Epoxy Composites 349

Reza Eslami-Farsani and Hossein Ebrahimnezhad-Khaljiri
12.2 Shape Memory Epoxy Polymers and their Composites 350
12.2.1 The Creation of Shape Memory Behavior into Epoxy 350
12.2.2 Shape Memory Behavior in Epoxy-Based Nanocomposites 354
12.2.3 Shape Memory Behavior in Epoxy-Based Composite Structures 358
12.2.4 Shape Memory Wires in the Epoxy Composites 360
12.3 Smart Epoxy Composite Coating 360
12.3.1 Carbon-Based Nanomaterials–Epoxy Coating 364
12.3.2 Clay-Based Nanomaterials–Epoxy Coating 365
12.3.3 Silica-Based Nanomaterials–Epoxy Coating 366
12.3.4 Layered Double Hydroxide-Based Nanomaterials–Epoxy Coating 367
12.3.5 Other Nanoparticles–Epoxy Coating 367
12.3.6 Polymer Micro-/Nanocontainer–Epoxy Coating 368
12.4 Self-Healing Epoxy Polymers and their Composites 371
12.4.1 Self-Healing Behavior 371
12.4.2 Intrinsic Healing System 372
12.4.3 Vascular Healing System 375
12.4.4 Microcapsule Healing System 377
12.5 Future Trends 380
12.6 Conclusion 380
References 381
xii Contents
13 Projects Using Composite Epoxy Materials: Applications,

Recycling Methods, Environmental Issues, Safety, and Future
Directions 395
Alencar Bravo and Darli Vieira
13.1 Introduction and Context of ECM Projects 395
13.2 Different Applications for ECMs 397
13.3 Safety and Environmental Issues of ECM Projects 400
13.4 Recycling Options for ECMs and Pollution Mitigation by
Early Design 405
13.5 The Future for ECM Projects and Conclusions 410
References 412
Index 421
1
Introduction to Epoxy Composites

Harikrishnan Pulikkalparambil 1 , Sanjay Mavinkere Rangappa 1 , Suchart
Siengchin 1 , and Jyotishkumar Parameswaranpillai 2
1
King Mongkut’s University of Technology North Bangkok, Department of Mechanical and Process
Engineering, The Sirindhorn International Thai-German Graduate School of Engineering (TGGS), 1518
Pracharat 1, Wongsawang Road, Bangsue, Bangkok 10800, Thailand
2 King Mongkut’s University of Technology North Bangkok, Center of Innovation in Design and Engineering
for Manufacturing, 1518 Pracharat 1, Wongsawang Road, Bangsue, Bangkok 10800, Thailand
1.1 Introduction
In the last two decades, one can observe a great increase in the replacement of
traditional materials with polymer composites in high-strength and lightweight
applications [1–3]. This is due to its high strength/weight ratio, toughness, and
thermal stability [4]. Several factors are associated with the composite performance,
such as filler properties, filler geometry, matrix properties, filler–matrix interac-
tions, filler orientation in the matrix, and the volume fraction of the filler [5]. The
matrix component of the composites can be thermoplastic, thermoset, or rubber.
Thermosetting polymers are widely used over others in engineering applications
due to their versatility and high performance. The epoxy resin was marketed in
the late 1940s, since then it is widely used for several industrial and commercial
applications. Its low shrinkage, better rigidity, good chemical and corrosion resis-
tance, remarkable adhesion properties, good thermomechanical properties, good
dielectric strength, etc., make it widely useful in engineering applications [6, 7].
Unlike polyester resins, epoxy can retain its mechanical and physical properties
under the influence of aggressive solvents. Also, epoxy resin will bond with almost
all materials such as stone, wood, glass, plastics, ceramics, and metals [8].
Epoxy resins are low-molecular weight materials that comprise oxirane/epoxide
rings as functional groups attached to their main chain [9]. The characteristics of
the epoxy resin make it suitable for reactivity against a wide range of curing agents.
Different types of epoxy resins are available such as diglycidyl ether of bisphenol-A
(DGEBA), cycloaliphatic epoxy resin, triglycidyl p-amino phenol, tetraglycidyl
diamino diphenyl methane, and novolac epoxy resins [10]. In addition, other
modified epoxy systems are available such as biobased epoxy, fluorine-containing
Epoxy Composites: Fabrication, Characterization and Applications,

First Edition. Edited by Jyotishkumar Parameswaranpillai, Harikrishnan Pulikkalparambil,
Sanjay M. Rangappa, and Suchart Siengchin.
© 2021 WILEY-VCH GmbH. Published 2021 by WILEY-VCH GmbH.
2 1 Introduction to Epoxy Composites
epoxy, phosphorus-containing epoxy, and silicon-containing epoxy. While the

curing agents are mainly catalysts or hardeners, the catalysts are tertiary amines
or Lewis acids, and their function is to initiate polymerization of the epoxy resin
to produce polyether structures [11]. The role of epoxy resin in the composite is to
transfer the force uniformly onto the filler and protect the integrity of the entire
composite system [12].
Epoxy resin with natural fibers, synthetic fibers, and other reinforced particles
has been extensively studied in recent decades [13]. Synthetic fiber-reinforced
epoxy composites are made of synthetic fibers such as glass, carbon, kevlar, and
aramid. Due to their lightweight, good strength, and good modulus, synthetic
fiber-reinforced epoxy composites are generally used in automobile and con-
struction applications. However, the recyclability of the synthetic fibers from the
composites after use is a concern. Recently, natural fibers are used in automotive
and construction industries due to their advantages, such as biodegradability, easy
availability, lightweight, cheap, simple processing, and good thermomechanical
properties. Extensive study has been done on epoxy composites based on natural
fibers such as kenaf, banana, jute, bamboo, and cotton [14–16]. Studies have
shown that they can replace glass and carbon fiber (CF) in epoxy composites for
semi-structural applications [14–17]. Furthermore, epoxy is the best resin that
can be used with either synthetic fiber or natural fiber [16, 18–22]. On the other
hand, the addition of micro- or nanofillers shows different behavior. For example,
the addition of clay fillers limits the plastic behavior of epoxy due to the rigid
clay behavior. Abdellaoui et al. [23] discussed the effect of clay loading on the
deformation of epoxy composites. The strength of the composites decreased with
the incorporation of clay. It was observed that at lower clay loading (5% and 10%),
the epoxy–clay interactions are weak owing to poor distribution. On the other hand,
at higher loading of 20 wt%, the clay particles agglomerate forming high-stress
concentration zones, which further weaken the composite strength. Thus, they
concluded that the incorporation of clay particles weakens the epoxy ductility and
degrades mechanical properties. Similarly, carbon nanotubes (CNTs) in epoxy were
reported to show poor dispersion with an increase in specific surface area. However,
the dispersion of CNTs in the epoxy matrix can be improved by chemical function-
alization, especially functionalization with amino group improved dispersion to a
large extent [24].
1.2 Manufacturing Methods for Fabrication of

Epoxy Composites
For the manufacture of epoxy-based composites, several methods were used in differ-
ent fields of application with the requirement of the final shape and size of the com-
ponents. Some of the most important methods used for the manufacturing of epoxy
composites are hand layup, vacuum bagging, vacuum-assisted resin transfer mold-
ing, autoclave, compression molding, pultrusion, and filament winding. All these
methods have their own advantages and disadvantages. The best selection of the
1.3 Experimental Techniques for the Characterization of Epoxy Composites 3
method gives the best result in any manufacturing industry. Different manufacturing
techniques used for the preparation of epoxy composites are given in Table 1.1.
1.3 Experimental Techniques for the Characterization of

Epoxy Composites
The detailed understanding of the epoxy composites is necessary for its effective uti-
lization in various application areas. Several characterization techniques have been
used to study the reinforcement effect of different fillers in epoxy matrices. Some
of the characterization techniques used for the characterization of epoxy compos-
ites are universal testing machine, dynamic mechanical analysis (DMA), differential
scanning calorimetry (DSC), rheology, thermogravimetry analysis (TGA), electron
microscopy, contact angle, and water absorption studies [47–50].
The rheological measurement is very helpful in analyzing the state of dispersion
and interfacial interaction of the nanoparticles with the epoxy matrix [51, 52].
Song et al. [52] studied the impact of dispersion of multi-walled carbon nanotubes
(MWCNTs) on the rheological properties of the epoxy composites. The authors
reported increased storage modulus, loss modulus, and complex viscosity with
the incorporation of MWCNTs. This implies that the MWCNT-based composite
exhibits a solid-like behavior. Kim et al. [53] studied the rheological properties
of surface-modified MWCNTs in the epoxy composite. The rheological studies
revealed that the modified MWCNTs in the epoxy matrix show higher storage
modulus, loss modulus, and shear viscosity when compared with the untreated
MWCNTs. This is because MWCNTs treated with acid, plasma, and amine intro-
duce functional groups onto the surface that imparts good dispersion and strong
adhesion between the MWCNTs and epoxy matrix. The least modulus and viscosity
were observed for the neat epoxy system. Park et al. [54] studied the rheological
properties of the acid-treated MWCNT-reinforced epoxy matrix composites. They
reported that the surface-treated MWCNTs composite showed good dispersion and
faster gel time. In another work, Zhu et al. [55] studied the fiber distribution and
interfacial interaction of 3-aminopropyltriethoxysilane (APTES)-modified carbon
nanofiber (CNF) in the epoxy composite. They observed a sharp increase in complex
viscosity and storage modulus at high temperatures due to the in situ reaction of
amine groups present in APTES with epoxy resin.
The DMA is used to study the viscoelastic properties of composites. Here, the
change in viscoelastic property of a material with respect to temperature or fre-
quency is measured to study the material behavior under dynamic conditions. The
storage modulus, loss modulus, and tan delta are the parameters observed from the
DMA measurements. These parameters are used to study the viscoelastic behavior
of the composite material [56]. The transition of the material from glassy to rub-
bery, i.e. glass transition temperature, can also be measured using DMA. In a recent
work, Yorseng et al. [50] studied the dynamic mechanical behavior of neat bioe-
poxy and kenaf/sisal fiber fabric-reinforced epoxy composites. The authors observed
a rapid drop in the storage modulus at the T g of the bioepoxy matrix. However, for
Table 1.1 Manufacturing techniques used in composite fabrication.
Manufacturing
S. No. methods Remarks References
1. Hand layup The advantages of using hand layup are design [25–28]
freedom and least expensive. The disadvantages are
the need for a greater number of cycles for fabrication,
skilled labor cost, risk of placement errors, molding of
complex parts with thickness variation, and poor
surface finish.
2. Vacuum The advantages of vacuum bag molding are better [29]
bagging finish, void free, and, possibility of using a heated
oven to accelerated consolidation. The disadvantages
include more complex and expensive compared to
hand layup, need to design the vacuum bag according
to component dimensions, and finally, the size of the
final component is limited to mold size.
3. Vacuum- The advantages of VARTM are the ability to [30–32]
assisted resin manufacture large complex parts, can be used to
transfer produce different component geometries, resin and
molding hardener can be stored separately and mixed just
before infusion, and low volatile organic compound
emission. The disadvantages of the VARTM process
are the difficulty in the reuse of bag, tube, sealing
tapes, and other consumables after one cycle, pressure
(both injection pressure and compressive pressure) is
limited in between vacuum pressure and atmospheric
pressure, leakage problems, less robustness, etc.
4. Solvent casting The advantages of solvent casting are simple [33]
fabrication process and no need for specialized
equipment. This technique limits the use of any
mechanical stress or high thermal processes to avoid
any degradation or side reactions. However, the
limitation of the solvent casting method is the use of
an external solvent that may affect
environment-friendliness and costs.
5. Autoclave The advantage is that it produces composites with [34]
closer control of thickness and lower void content.
The limitation of this process is that the component
size may be limited to the autoclave size.
6. Compression The advantages of compression molding are easy [35, 36]
molding processing, low cost, and minimum waste. The
disadvantage of using compression molding is it is
limited to small-scale industries due to the
time-consuming process. Also, the compression
molding technique requires highly trained manpower
to operate the processes.
7. Pultrusion The advantages of pultrusion are the unlimited length [37, 38]
of the products, smooth surface, and continuous
production. The disadvantages include limited size in
the transverse direction, reinforcement in only one
direction, and expensive.
(Continued)
1.3 Experimental Techniques for the Characterization of Epoxy Composites 5
Table 1.1 (Continued)
Manufacturing
S. No. methods Remarks References
8. Filament The advantages of filament winding are higher [39, 40]

winding reinforcement levels (up to 70% or more to improve
mechanical strength), tailoring orientation of fibers,
and large component fabrication is possible. The
disadvantages are heavy investments and limited
design and shape.
9. Low shear These are batch-type mixers that are versatile to be [41]
liquid batch suitable for all types of processing conditions such as
mixer mixing sequence, mixing temperature, and mixing
10. Internal mixer time. However, the limitation of these mixers is time
consumption.
11. Rheo mixer
(RMX)
12. Extrusion The advantages of using extruders are low cost, good [42]
heat transfer, good mixing, high production, and good
surface finish. The disadvantages are size variance
and product limitations.
13. Three-roll mill The main advantage of the three-roll mill is good [43–45]
dispersion. The fillers can achieve highly intercalated
or exfoliated structure.
14. Resonant The main advantage of RAM mixers is uniform [46]
acoustic mixer mixing, unlike the batch and continuous mixers
where localized mixing near the region of mixing
blade tip is observed.
the composites, the drop in storage modulus at the T g is marginal due to reinforce-
ment of sisal and kenaf fibers with bioepoxy matrix. Matykiewicz et al. [57] studied
the thermomechanical properties of epoxy composites filled with glass fiber. The
authors reported an improvement in the storage modulus of the epoxy composite
with the incorporation of glass fiber, due to better dispersion of glass fiber in the
epoxy matrix. In another work, Chateauminois et al. [58] studied the plasticization
of unreinforced and epoxy/glass fiber-reinforced unidirectional composites using
DMA. The samples of reinforced and unreinforced composites were both unaged
and aged by immersion in water. The composite samples were dried in an air oven
immediately after immersion. The results of the samples were compared for change
in plasticization after aging. The authors observed a change in plasticization for
reinforced composites after aging. This is due to the trapping of water in the voids
generated at the fiber/matrix interface because of hygrothermal aging. In a similar
work, Xian and Karbhari [59] investigated the moisture uptake and aging of a room
temperature cured epoxy system using DMA. The plasticization was observed in the
aged samples.
The DSC is mostly used for the measurement of T g and the cure kinetics of the
epoxy thermoset [60]. The cure kinetics of epoxy composites and the degree of cure
is dependent on the curing temperature [61, 62]. High cure temperature accelerates
the curing reaction and hence decreases the cure time. The T g behavior of compos-
ites with different filler loadings may be used to understand the interaction between
the polymer and fibers. The addition of fillers in epoxy composites may have strong
effects on the T g [61]. Gojny and Schulte [63] reported that the T g of the compos-
ites may vary with the addition of CNT, and the change is more noticeable with
functionalization. Also, the composites with a strong filler polymer interface show
improved T g . Kang et al. [64] studied the DSC of functionalized nanosilica particles
obtained using the sol–gel process in epoxy composites. An improvement in the T g
was observed for the composites with strong interfacial interactions.
The thermal stability of epoxy composites plays an important role in determining
the maximum temperature up to which the material is safe for practical appli-
cations. In TGA, the mass of a sample is monitored against temperature using
a thermo-balance [65]. The weight loss at a specific temperature determines the
amount of degradation, and the temperature at which maximum weight loss
is observed shows maximum degradation temperature. Also, TGA is useful for
determining the composition of lignocellulosic biomass such as lignin, α-cellulose,
and hemicellulose contents [66, 67]. TGA is also used for the fiber and void content
analysis in composites. Yee and Stephens [68] showed a fast and precise method
to study the graphite fiber content in epoxy composites using TGA. Nowadays,
hydrogen fuel in automotive has attracted most of the people due to the depletion of
fossil fuels. However, the storage of hydrogen fuel needs to be taken care of due to
its very high pressure and flammability. Very recently, Zhang et al. investigated the
thermal stability of CF-reinforced epoxy composites taken from the outer material
of hydrogen fuel storage tank [69]. TGA and Fourier transform infrared analysis
(FTIR) can be used to study the pyrolysis of epoxy composites. The TGA is used to
analyze the weight loss at elevated temperatures, while FTIR is used to measure
constituents and functional groups in the produced gases. They reported that the
decomposition of epoxy composite takes place between 277 and 477 ∘ C [70, 71].
FTIR spectroscopy is a form of the vibrational spectroscopic technique commonly
used to determine the functional groups present in the composites [72]. FTIR is also
used to measure the curing reaction, phase separation, and aging with the assess-
ment of bands [73]. The FTIR peaks are obtained in the range between 4000 and
400 cm−1 . The oxirane ring in the epoxy resin is observed at 915 cm−1 , which corre-
sponds to C–O deformation, and the peaks at 3050 cm−1 correspond to stretching of
methylene groups in the epoxy ring. Table 1.2 shows characteristic FTIR peaks of
DGEBA epoxy resin.
1.4 Properties of Epoxy Composites

1.4.1 Mechanical Properties
The mechanical properties of epoxy composites are an important topic in shaping its
efficient use in any application area. The factors that affect the mechanical properties
Table 1.2 Characteristic bands of DGEBA.
Band (cm−1 ) FTIR peak assignment
≈3500 O–H stretching

3057 C–H stretching vibrations of the oxirane ring
2965–2873 C–H stretching vibrations in epoxy resin
1608 C=C stretching vibrations of aromatic rings
1509 C–C stretching vibrations of aromatic rings
1036 C–O–C stretching vibrations of ethers
915 C–O stretching vibrations of oxirane group
831 C–O–C stretching vibrations of oxirane group
772 CH2 rocking
Source: María González et al. [73]. IntechOpen. CC BY 3.0.
of filler-reinforced epoxy composites are volume fraction of filler, filler aspect ratio,
filler orientation, and filler–matrix interfacial adhesion [74]. The mechanical proper-
ties of natural fiber composites can be improved when it is used along with synthetic
fibers [75]. In other words, the hybridization of natural fiber and synthetic fiber
leads to improved mechanical properties due to the synergetic effects of both the
fibers. Fiore et al. [76] studied the effect of alkali (NaOH) treatment on kenaf fibers.
They reported that the alkali treatment resulted in improved mechanical strength by
reducing the polymer chain mobility and enhancing the stress transfer. However, the
immersion time in NaOH had an unfavorable effect on the mechanical properties.
The particle size of fillers may also affect the mechanical properties. For example,
Wang et al. [77] showed the effect of particle size of graphene nanoplatelets on the
mechanical properties of epoxy composites. Moderate increase in strength and mod-
ulus is observed when smaller particles are used. On the other hand, larger particles
improve the modulus remarkably but reduce the strength. This is due to the rein-
forcement effect of larger particles, but they have poor interfacial interaction with
the epoxy matrix. In an interesting work, Gojny et al. [24] schematically described
several mechanisms during the failure of CNT-modified epoxy matrix as shown in
Figure 1.1. The different failures occurring on the CNTs during the application of
tensile force are pullout, breakage, pullout of inner tube, and bridging or partial
debonding at the interfaces.
The impact strength/resistance of a composite is the energy needed to break any
material. In other words, the impact strength of a material is its ability to resist the
applied stress at high speed. Many factors such as voids, sharp edges of fillers, filler
agglomeration, and weak filler–epoxy interface may lead to stress concentrated areas
that may cause failures in the form of cracks by the application of applied stress
[78, 79]. One way to improve the impact strength is by the addition of dispersants or
coupling agents [80]. The addition of dispersants reduces filler agglomeration that
could otherwise act as a stress concentration point. Devendra and Rangaswamy [81]
(a) (b) (c) (d) (e)
Figure 1.1 Schematic representation of failure types in epoxy/CNT composites: (a)

undamaged CNT, (b) CNT pullout, (c) CNT breakage (very good CNT–epoxy interaction), (d)
telescopic pullout damaging outer tube and pullout damaging inner tube, and (e) bridging
and partial debonding at interface. Source: Gojny et al. [24]. © 2005, Elsevier.
reported that the filler content higher than optimum has an adverse effect on the
impact resistance of a composite due to agglomeration of fillers.
The interfacial shear stress (IFSS) measures the degree of interfacial strength
between the filler and the epoxy matrix. Wang et al. [82] studied IFSS measure-
ments of Ag nanoparticles and graphene oxide (GO)-deposited CF-reinforced epoxy
composites. The authors reported that the IFSS improved from 46.8 to 87.1 MPa for
the epoxy composites. The presence of Ag nanoparticles was observed to increase
the surface roughness of the fiber and the matrix, which provides better interlocking
between the fiber and the matrix. While the incorporation of GO greatly improves
the wettability and interfacial adhesion between the CF and polymer matrix that
leads to improved shear strength (Figure 1.2). Godara et al. [83] studied the effect of
CNTs on the IFSS of glass fiber-reinforced epoxy composites. It was observed that
CNTs improve the IFSS irrespective of its location in the composites. However, as
Crack Ag NPs
Carbon
Epoxy
fiber
Debonding Debonding GO
Untreated CF CF/Ag CF/Ag/GO
Figure 1.2 Scheme showing failure mode of untreated CF-modified epoxy, CF/Ag-modified
epoxy, and CF/Ag/GO-modified epoxy. Source: Wang et al. [82]. © 2017, Elsevier.
Figure 1.3 Schematic representation IFSS increase

of CNTs on different locations in the
composite and its effect on IFSS.
Source: Godara et al. [83]. © 2010,
Elsevier.
shown in Figure 1.3, the maximum improvement of IFSS is observed for composites
with CNTs on the surface of the glass fiber.
1.4.2 Dielectric Properties

The dielectric constant and the dissipation factor are the two important parameters
in measuring the dielectric properties [84]. The dielectric constant measures the
ability of the material to store charge, while the dissipation factor is the energy dis-
sipated by a dielectric. These are measured as a function of frequency of alternating
current by placing the composite material between the plates of a condenser and
measuring the impedance [85, 86]. The dielectric constant of epoxy resin is very
low (<10) to be useful in practical applications [87]. Incorporating an adequate
amount of fillers may improve the dielectric properties to some extent. However,
higher loading may affect the mechanical properties of the composite [88–90]. In an
interesting work, Singha and Thomas [91] studied the dielectric properties of inor-
ganic filler (TiO2 , ZnO, and AI2 O3 )-incorporated epoxy composites. It was observed
that the permittivity and tan delta values of the nanocomposites were lower than
those of the micro-composites and unfilled composites. In another work, Kuo et al.
[92] prepared epoxy composites using self-synthesized barium titanate (BaTiO3 ),
commercial BaTiO3 , and Pb(Mg1/3 Nb2/3 )O3 ceramic particles. It was observed that
the self-synthesized ceramic particle BaTiO3 exhibits a dielectric constant of 44
compared to 27 and 24 for commercial BaTiO3 and Pb(Mg1/3 Nb2/3 )O3 composites.
This is due to the large ceramic aggregates formed in the epoxy composites by
self-synthesized BaTiO3 . In another study, Wan et al. [93] reported the dielectric
properties of DGEBA–RGO/epoxy composites, where DGEBA–RGO was prepared
by grafting DGEBA molecules on reduced graphene oxide (RGO) sheets. The
DGEBA–RGO/epoxy composites showed an improved dielectric constant of ∼32.
This was attributed to better compatibility arising due to grafting of DGEBA and the
better contact of RGO sheets making a pathway for suppressing the dielectric loss
effectively. In one of the works, Jlassi et al. [94] reported that a very small amount
of diazonium-modified clay-polyaniline nanofiller (B-DPA/PANI) in the epoxy
matrix can improve the tensile strength (0.1 wt%) and dielectric constant with the
incorporation as low as 0.5 wt%. This is due to the good dispersion of the nanofiller
in the epoxy matrix.
1.4.3 Water/Moisture Absorption

Water absorption of a material maybe defined as the percentage of water uptake in
a given unit time at a specific temperature. It is calculated by measuring the change
in weight with respect to its original weight after a given time. The weight gained at
saturation is the final weight.
Initial weight of sample-Final weight of sample
Water uptake (%) = × 100
Initial weight of sample
The rate of water uptake can be measured by calculating the diffusion coefficient of
the composites [95]. The following equation can be used to calculate the coefficient
of diffusion:
( )
kh 2
D=π
4Mn
One of the main limitations of epoxy resin and its composites is its high water
absorption. The water uptake may adversely affect the T g , modulus, strength, and
toughness due to the degradation of the epoxy thermoset [73]. It also generates inter-
nal stresses due to swelling and causes delamination of the filler or other defects
in composites. In general, the main concern with natural fiber composites is their
high moisture intake due to the presence of hydroxyl groups in the fiber, which
reduces the compatibility between the fiber and the epoxy matrix [96]. In fact, the
fiber–matrix interfacial strength may be reduced, which in turn will decrease the
mechanical performances of the composites. In few studies, it was observed that
the hybridization of fibers in the composite may improve the mechanical and water
absorption properties [97–99]. For example, Maslinda et al. [100] studied the effect
of water absorption on the mechanical properties of woven kenaf, jute, and hemp
fiber-based hybrid epoxy composites. The authors reported that the mechanical and
water-resistant properties of the composites were improved with hybridization.
The water absorption is observed to be higher for natural fiber-reinforced com-
posites when compared to synthetic fiber-reinforced composites [101, 102]. There-
fore, the hybridization of natural fiber and synthetic fiber reduces the water uptake
tremendously. Sanjay and Yogesha [102] studied the water absorption behavior of
jute, kenaf, and E-glass woven fiber-reinforced epoxy composites with different lay-
ering sequences. The authors reported a reduction in water absorption behavior with
the hybridization of natural and synthetic fibers. Venkateshwaran et al. [103] stud-
ied the water absorption rate of sisal and banana fiber composites. They observed a
reduction in the rate of water absorption after hybridizing the sisal fiber (50%) with
banana fiber.
The wetting of fibers or fillers plays an important role in reducing the water
absorption because wetting improves the adhesion of the filler with matrix
[104, 105]. The addition of a small amount of nanoclay (c. 3–5 wt%) in epoxy
composites exhibits improved barrier properties [106, 107]. Becker et al. [108]
studied water absorption in nanoclay-filled tetrafunctional tetraglycidyldiamino
diphenylmethane (TGDDM) and DGEBA resin systems. It was evident from the
results that nanoclay-filled composites showed lower water absorption when
compared to neat epoxy resin. However, the rate of diffusion with the change in
nanoclay concentration is observed to be unaffected. In an interesting work, Mohan
and Kanny [109] reported the water barrier properties of sisal fiber-modified epoxy
composites and nanoclay-filled sisal fiber-reinforced epoxy composites. After water
absorption, the tensile and wear properties of sisal fiber composites detrimentally
decreased. However, after the addition of nanoclay to sisal fiber composites, the
tensile and wear properties are least affected. This is due to the barrier property of
nanoclay that stops the water from entering the composites.
1.4.4 Morphology
The morphology of composites plays an important role in identifying the failure
mechanisms. For example, electron microscope is used to analyze the existence
of voids, agglomeration, and dispersion of fillers [110, 111]. In an interesting
study, Saba et al. [111] prepared hybrid epoxy composites containing kenaf and oil
palm empty fruit bunch fiber (OPEFB) fillers that showed improved mechanical
properties. The morphology study revealed that the addition of 3% OPEFB filler
into epoxy/kenaf composites was observed to improve the interfacial bonding
between the fiber and matrix. Also, the addition of OPEFB fiber reduces void
contents, fiber pullout, and fiber protruding and tearing on the composites. Oks-
man et al. [112] studied the morphology of unidirectional sisal/epoxy composites.
Figure 1.4a,b shows scanning electron microscopy (SEM) images of fractured
surface of sisal/epoxy composites. Here, the fiber pullout and imprints are visible.
Figure 1.4c,d shows the optical microscopy images of the composites. The figures
show fiber distribution and horseshoe-shaped technical fibers. Atomic force
microscopy (AFM) is also a powerful tool to characterize surface morphology and
(a) (c)
(b) (d)
Figure 1.4 (a and b) SEM image of sisal/epoxy fracture surface shows fiber pullouts and
imprint of the fiber on epoxy surface, (c and d) optical microscopy of sisal/epoxy composites
shows horseshoe structure and voids in the fiber–epoxy interface. Source: Oksman et al.
[112], Reproduced with permission from Wiley, License Number:4847180686936.
30.0 60.0° 30.0 60.0°
30.0° 30.0°
20.0 20.0
0.0° 0.0°
10.0 10.0
0 0
0 10.0 20.0 30.0 0 10.0 20.0 30.0
0 hr 12 hr
30.0 60.0° 30.0 60.0°
30.0° 30.0°
20.0 20.0
0.0° 0.0°
10.0 10.0
0 0
0 10.0 20.0 30.0 0 10.0 20.0 30.0
36 hr 61 hr
5.00 60.0°
30.0°
0.0°
2.50
0
0 2.50 5.00
Figure 1.5 AFM image showing debonding occurred during hygroscopic treatments of
carbon fiber-reinforced composite. Source: Wang and Hahn [114], Reproduced with
permission from Elsevier, License Number:4847180982493.
thickness of nanosized fillers in epoxy composites. George and Verpoest [113]

characterized the untreated and silane-treated fiber using AFM and observed that
the surface of the treated fibers is rougher than that of the untreated fibers. In
another work, Wang and Hahn [114] studied the effect of hygrothermal processes
on the interfacial properties of CF-reinforced epoxy composites. The AFM was
used to investigate the debonding of fibers. Figure 1.5 shows the AFM image of
debonding in hygroscopic treated composites at different time intervals.
References 13
1.5 Conclusion
In this chapter, an overview of the manufacturing, characterization, and properties

of the epoxy composites is briefly discussed. It is worth to point out that the applica-
tions of epoxy composites are widely accepted in all areas of manufacturing indus-
tries such as automotive, aerospace, construction, oil and gas, and marine owing to
their excellent heat and solvent resistance, high thermomechanical properties, high
specific strength, good adhesiveness, lightweight, and low cost. Epoxy composites
also find applications in printed circuit boards (PCBs), electromagnetic shielding
(EMI), supercapacitors, etc. The high performance of the composites is generally
achieved by the incorporation of fibers, organic fillers, and inorganic fillers. Further-
more, the addition of thermoplastic copolymers may phase separate into different
phase morphologies which may tailor the performance of the epoxy composites.
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23
Synthesis and Manufacturing of Epoxy Composites

Turup P. Mohan and K. Kanny
Durban University of Technology, Composite Research Group, Department of Mechanical Engineering,
Steve Biko Campus, Steve Biko Road, Berea, Durban 4000, South Africa
2.1 Introduction
Epoxy resins are a thermosetting synthetic polymer which are basically composed
of two substances known as resin and hardener. The main purpose of epoxy is to
be used as an adhesive due to its high durability. Epoxy resin adhesive forms an
excellent bonding agent. The bonding of the resin can be developed to yield sev-
eral different products, each with its own unique application. Epoxies are typically
used to fabricate high-performance composites with superior mechanical properties,
resistance to corrosive liquids, and environments. Epoxies are also used to achieve
good electrical properties, good performance at high temperature, and good adhe-
sion to the substrate.
2.2 History of Epoxy Resin

The first commercial possibilities for epoxy resins were realized in Switzerland
by Pierre Castan of De Trey Freres and in the Unites States by Sylvan Greenlee of
DeVoe and Raynolds. In 1936, Castan produced a bisphenol-A-based epoxy resin via
reaction with epichlorohydrin and subsequently prepared a thermoset composition
after reaction of the resin with phthalic anhydride. The use of the hardened resin
was foreseen in dental products, but initial attempts to market the resin were
unsuccessful. The patents were licensed to CIBA AG of Basel, Switzerland (now
CIBA-GEIGY), and in 1946, the first epoxy adhesive was shown at the Swiss Indus-
tries Fair [1]. During 1939, Sylvan Greenlee produced a high molecular weight resin
from bisphenol-A and epichlorohydrin which was subsequently esterified with
unsaturated fatty acids to provide an air-drying coating. His first patent was issued
in 1948 [2]. In 1949, production of very high molecular weight thermoplastic poly-
mers from bisphenol-A and epichlorohydrin was reported in 1949 using a one-step
or two-step synthesis route, i.e. starting with epichlorohydrin and bisphenol-A in
Epoxy Composites: Fabrication, Characterization and Applications,

First Edition. Edited by Jyotishkumar Parameswaranpillai, Harikrishnan Pulikkalparambil,
Sanjay M. Rangappa, and Suchart Siengchin.
© 2021 WILEY-VCH GmbH. Published 2021 by WILEY-VCH GmbH.
24 2 Synthesis and Manufacturing of Epoxy Composites
a 1 : 1 mole ratio or utilizing a purified diglycidyl ether of bisphenol-A resin and a

stoichiometric quantity of bisphenol-A in a solution polymerization [3]. Aerospace
was the first commercial field that epoxies could penetrate within the early 1950s.
It took more than two decades for epoxies to get its exposure [4]. Epoxies have
made their way to residential applications and as a flooring option for parking lots
during 1970s. This as a flooring substitution has shown prolonged longevity, ease of
clean, and scratch proof properties. Epoxy is now a global compound with a dozen
of breakthroughs that have occurred over the century and has now become the
world’s best and most used compounds [5]. Today epoxy adhesives are sold in local
hardware stores, usually used as a binder under countertops or floor coatings [6].
2.3 Types of Epoxy Resins
2.3.1 Bisphenol-A Epoxy Resin

Production of epoxy resins is achieved by fusing epichlorohydrin and bisphenol to
get bisphenol-A diglycidyl ethers, to produce polyethers together with glycidyl end
groups that at room temperature have semi-crystalline materials. It is processed by
increasing the ratio of bisphenol-A:epichlorohydrin [7]. Figure 2.1 shows the final
product of bisphenol-A epoxy resin (chemical reaction of bisphenol-A and epichloro-
hydrin).
Raw materials: Materials that are used to make bisphenol-A epoxy resin are
epichlorohydrin and bisphenol-A [8].
Production: Bisphenol-A epoxy resin is produced by condensation of acetone with
2 equiv of phenol. Hydrochloric acid or a sulfonated polystyrene resin is used to
speed up the reaction. When acid is used as a catalyst, condensation of phenol with
acetone happens [9].
2.3.2 Bisphenol-F Epoxy Resin

In this type of resin, viscosity is low and mean epoxy content per gram is high than
bisphenol-A and chemical resistance increases once cured. Bisphenol-F undergoes
CH3
CH3
C
C
OH
CH3
O CH3 CH
CH2 CH2 O
CH2 CH CH2 O O
CH2
O
CH2 CH
Figure 2.1 Chemical structure of bisphenol-A type epoxy resin.

2.3 Types of Epoxy Resins 25
H
H
C
C OH
H
O H CH
CH2 CH CH2 O CH2 CH2 O
O
CH2
O
CH2 CH
Figure 2.2 Chemical structure of bisphenol-F epoxy.
epoxy resin formation similar to bisphenol-A. Figure 2.2 shows the chemical struc-
ture of bisphenol-F epoxy resin.
Raw materials: Phenol, formaldehyde, and phenol paraben methanol dehydration
catalyst [10].
Production: This epoxy resin is produced by reacting phenol and formaldehyde.
This reaction takes place in the presence of a catalyst which is acid plus water and
the unreacted phenol from the product to give a crude bisphenol-F and removing
the acid catalyst. A part of the crude bisphenol-F is distilled to give a highly pure
bisphenol-F. A distillate has a binuclear moiety content that is not <95% by weight
and a novolac phenol resin, as a still-bottom product, having a binuclear moiety con-
tent that is not more than 15% by area. To give bisphenol-F for general use, highly
pure bisphenol-F is mixed with the remaining crude bisphenol-F [9].
2.3.3 Phenol Novolac Epoxy Resin

Yielding epoxidized novolacs is achieved by the phenol reaction among subsequent
glycidylation and formaldehyde, along with epichlorohydrin, like epoxy cresol
novolacs (ECN) and epoxy phenol novolacs (EPN). The following resins compared
to solid resins are exceptionally viscous and normal including epoxide function-
ality. When there is high epoxide functionality, an exceptionally cross-linked
polymer network leading to chemical resistance and high temperature with low
pliability is produced [11, 12]. Figure 2.3 shows the chemical structure during the
response of phenols among subsequent glycidylation and formaldehyde, along with
epichlorohydrin to produce phenol novolac epoxy resin.
Raw materials: Phenolic novolac resin and epichlorohydrin [13].
Production: Novolac epoxy resin is formed as a result of the reaction between phe-
nolic novolac resin and epichlorohydrin. A highly cross-linked polymer network is
formed by the high epoxide functionality of these resins showing high temperature
and chemical resistance with low flexibility [8]. Novolac resins prepared by reacting
phenolic novolac resin and epichlorohydrin are then reacted with epichlorohydrin
and 30% NaOH solution and then later added to the reaction vessel over a period
of 2.5 hours to conduct the epoxidation process; a 2 l glass reactor equipped with a
thermometer, reflux condenser, and stirrer is required [13].
O
O
CH CH2
O CH CH2
CH2 CH2
CH2 CH O
Figure 2.3 Chemical structure of phenol novolac epoxy.
O O
H
O CH CH2 CH2 CH O
O N C N O
O CH CH2 CH2 CH O
H
Figure 2.4 Cycloaliphatic epoxy resin structure.
2.3.4 Cycloaliphatic Epoxy Resin

This class of resin epoxy at room temperature displays low viscosity and offers rel-
atively much higher temperature resistance than the aliphatic epoxy diluents. A
class applicable is cycloaliphatic epoxy resin, containing the molecule about a single
or more cycloaliphatic rings (e.g. 3,4-epoxycyclohexylmethyl-3,4-epoxycyclohexane
carboxylate). However, the rate of reaction is less corresponding to the other classes
of epoxy resins, and it is required to normally cure with high temperatures using
suitable accelerators. The ultraviolet (UV) stability is improved since aromaticity is
not in these materials [11, 14]. Figure 2.4 shows the chemical reaction that produces
cycloaliphatic epoxy resin.
Raw materials: Cyclohexenylmethyl and peracetic acid.
Production: Cycloaliphatic epoxy resin is formed by reacting 30-cyclo-
hexenylmethyl 3-cyclohexenecarboxylate with peracetic acid. This epoxy resin
has an aliphatic backbone and a fully saturated molecular structure [8].
2.3.5 Epoxy Resin Diluents

Formation of resin diluents is made with polyols or glycidylation of aliphatic
alcohol. Creating materials could be difunctional (e.g. butanediol diglycidyl ether),
monofunctional (e.g. dodecanol glycidyl ether), or with greater functionality (e.g.
trimethylolpropane triglycidyl ether). At room temperature, these resins show
typically low viscosity (10–200 mPa s) and they are termed “reactive diluents.” They
are not usually used alone but instead used to reduce or increase the viscosity of
other epoxy resins. This gives rise to the term “modified epoxy resin” to categorize
those containing viscosity-lowering reactive diluents [15, 16].
Raw materials: Glycidylation of aliphatic alcohols or polyols.
2.4 Curing 27
Figure 2.5 Glycidylamine epoxy resin CH3 CH3

structure. O O
O O
CH3 CH3
Production: Epoxy resin diluents are obtained from glycidylation [8]. Mono-epoxy
compounds and di/polyfunctional epoxies are epoxy resin diluents. Non-reactive
diluents compounds are not chemically bound into the cross-linked network; these
cured formulations that contain such materials usually show less chemical resis-
tance. In both classes, the existence of the epoxide group(s) permits the diluent to
interact with the resin and curing agent, to allow the diluent to form a chemical
cross-linked network structure [17].
2.3.6 Glycidylamine Epoxy Resin

Reaction between aromatic amines and epichlorohydrin results in glycidylamine
epoxy resins which are higher functional epoxies. The important grades of indus-
trial epoxies are triglycidyl-p-aminophenol (functionality 3) and N,N,N ′ ,N ′ -
tetraglycidyl-bis-(4-aminophenyl)-methane (functionality 4). At room temperature,
the resins range from low to medium functionalities thereby making it easier
to process when compared to ECN or EPN resins. The combination of higher
reactivity, high-temperature resistance, and mechanical properties of the cured
network structure results them an important material for aerospace composite
materials [18]. Figure 2.5 shows the glycidylamine epoxy resin chemical structure.
Raw materials: Glycidylamine is composed of aromatic amine and
epichlorohydrin.
Production: This epoxy resin is formed due to the reaction of two raw materials,
aromatic amine and epichlorohydrin [8]. Glycidyl epoxy resins are created using
bisphenol-A and are reacted with epichlorohydrin.
2.4 Curing
Epoxy resins may be cured using a variety of curing agents. Generally, any compound
that has a reactive hydrogen atom or hydroxyl group can react with the epoxide
groups of the epoxy resin. These curing agents could be amines, polyamides, car-
boxylic acids, anhydrides, imidazoles, or amide-amines [19]. It is possible to control
the cure rates to match processors through proper selection of hardeners and cata-
lysts. Since epoxy has a higher viscosity than resin, a post cure at higher temperature
is suggested to achieve superior mechanical properties.
2.4.1 Curing Agents

Curing agents or hardeners play a significant role in the curing kinetics, gel time,
extent of curing (crosslinking), viscosity, the characteristics of the curing products,
and curing processors [20, 21]. In general, there consists of three different types of
curing agents. Compounds containing hydrogen and their derivatives are the first
type. Anionic and cationic initiators are included in the second type of curing agents.
They are used to catalyze the homopolymerization of epoxy resins. The third would
be latent curing agents [22]. The curing agents are discussed in detail.
2.4.1.1 Polyaddition Reactions (Active Hydrogen Compounds)

Active hydrogen-based compounds are the most widely used, and these undergo
polyadditions through a compound that contains active elements of epoxy group
which are hydrogen and the terminal carbon, with the epoxide being stabilized into
a hydroxyl group.
Amines
Some of the factors required that affects the gel time of amine-based hardeners are
the loading of amine and the type of amine of epoxy resin used. Glycidyl ether is
a type of resin that is most popular, which can easily cure at room temperature.
Glycidyl-ester type cures faster compared to glycidyl ether type. Figure 2.6 shows
the different chemical constitutions of the different types of amines. Aliphatic and
aromatic amines are the classification groups of amines, due to the types of hydro-
carbons involved. Figure 2.6 shows the chemical structure of aliphatic amines.
Aliphatic Amine
This type of amine commonly has the following properties:
● Cures at room temperature.
● Final product has a strong and good bonding properties.
● Heat resistance of about 100 ∘ C.
● Curing at high temperatures can improve the properties of aliphatic amines.
120 ∘ C is the maximum heat deformation temperature of cured product.
● Aliphatic amine contains a stronger basicity than aromatic amine.
Aromatic Amine
● They are highly resistant to heat and chemicals compared to that of aliphatic
amine which only ranges up to 100–150 ∘ C.
● Aromatic amine has strong mechanical and electrical properties.
● They have a strong resistance against chemicals, especially alkalis. This property
makes them to be highly resistant to solvents and also a good curing agent.
● With the help of steric hindrance by the aromatic ring, it can cure at slow rate at
room temperature.
● Figure 2.7 shows the chemical structure of a typical aromatic amine.
2.4.1.2 Polyamide and Polyamine

Polyamine is an organic compound which is composed of amino functional groups;
especially such compounds are formed by decomposition of proteins. Figure 2.8
shows the chemical structure of polyamide.
2.4 Curing 29
O NH2
CH3 n O m
Diamine:
H2N NH2
O n
CH3 CH3
CH3
Triamine:
O
H2 N NH2
x y
H2N NH2
O n O m
CH3 CH3
R
Polyamine:
NH2
CH3
Figure 2.6 Chemical structure of amines.

Figure 2.7 The chemical structure of aromatic amine.
••
N
CH3
H Figure 2.8 Chemical structure of polyamide.
(CH2)5
● The chemical reaction between dimer acid and polyamine forms polyamide.
● Primary and secondary amines are used to build up their molecules. Average
heat generation and base temperature allow the curing of polyamide amine and
bisphenol-A type epoxy resin when they react together.
● Pot life is relatively long due to its slow curing process. The molecules of
polyamide develop immense hydrocarbon moiety, a rigid thermosetting polymer
that is highly plasticized when cured in the epoxy resin.
● Excellent in shock resistance, with high compressive, bending, and tensile
strengths while being rigid and strong.
2.4.1.3 Secondary and Tertiary Amines

Tertiary amine is a polymerization catalyst, and it does not form any additional
reaction with resin. The types of curing agents dictate the loading during the cur-
ing process (i.e. loading of these amines is not constant) [23]. Figure 2.9 shows the
chemical structure of secondary and tertiary amines.
● Some of the factors that are influenced by the curing temperature are heat gener-
ation, properties of the cured resin, and curing speed.
● Paints and adhesives are of tertiary amines.
● It is used as an accelerator for polyamide and polyamine curing agents but is not
useful as a curing agent itself.
2.4 Curing 31
Figure 2.9 Chemical structure of (a) secondary amine H

and (b) tertiary amine.
••
N
R1 R2
(a)
RII
R RI
(b)
OH CH3
N N CH2 CH CH2 O C O CH2 CH CH2 N N
CH3 OH
Figure 2.10 Chemical structure of imidazole.
2.4.2 Anionic and Cationic Initiators

Anionic polymerization of epoxides is reduced by metal hydroxides, secondary and
amines. The molecular weight of the polymer increases as the polymerization pro-
gresses; this is called stepwise polymerization. Figure 2.10 shows the chemical reac-
tion that produces imidazole.
Type of agent categorized under anionic and cationic initiators is:
2.4.2.1 Imidazole (Anionic Polymerizing)

● Are well known as a good curing catalyst or agent.
● It has application in compositions of resin such as casting materials and filling
materials in one-part thermosetting coating adhesives.
● They have a longer pot life.
● Higher heat resistance and cure faster.
2.4.2.2 Polymercaptan
This type of curing agent functions at a low temperature (0 to −20 ∘ C) range.
Sometimes, tertiary amine is added as an accelerator. Polymercaptan rapidly
cures and attains average strength in 10–30 minutes while having a life span of
2–10 minutes [24]. Figure 2.11 shows the chemical formula of liquid polymercaptan
curing agent.
R O C3H6O CH2CH(OH) CH2 SH

m
n
Figure 2.11 Chemical formula of liquid polymercaptan curing agent.
CH2 Figure 2.12 Chemical structure of alicyclic anhydrides.
CH2 CH2
2.4.2.3 Anhydrides
While producing a small quantity of heat, these cured resins also emit controlled
mechanical, electrical, and chemical properties. Insolating coating for condensers
and casting uses solutions in a liquid anhydride.
2.4.2.4 Canhydrides
These are generally solid. This is popular in powder paints for uses in powder mold-
ing. Canhydrides are used for insulating the coating of condensers and casting. They
are the solution in liquid anhydrides.
2.4.2.5 Alicyclic Anhydrides

Most commonly used anhydrides fall into this section. Tetrahydrophthalic anhy-
dride, methyltetrahydrophthalic anhydride, hexahydrophthalic anhydride, methyl
nadic anhydride, and methylhexahydrophthalic anhydride are the principal curing
agents. Figure 2.12 illustrates the chemical structure of alicyclic anhydrides [25].
2.4.2.6 Aliphatic Anhydrides

The reaction between aliphatic dibasic acid molecules is known as dehydration
condensation which forms polycarboxylic anhydrides [23]. It can be used alone
or with other anhydrides in casting resin and curing agents known as powder
paints because it produces amazing thermal shock resistance and flexibility.
Aliphatic dibasic molecules react together by dehydration condensation. Tertiary
amine is curing accelerators which are boric acid ester, organic metal compounds,
Lewis acid, organic metal salts, or imidazole. The chemical structure of aliphatic
anhydride is shown in Figure 2.13.
2.4.3 Latent Curing Agents

Epoxy resin compositions which have outstanding storage stability at atmospheric
conditions are brought by latent curing agents, resulting curing at common and sub-
lime temperatures. Other elements used to cure are light, pressure, and heat which
cures others rapidly.
2.4 Curing 33
Figure 2.13 Chemical structure of aliphatic RI O RII

anhydride.
C C
O O
Figure 2.14 Chemical structure of boron CH2

trifluoride–amine complex.
BF3 · NH2 CH
CH2
2.4.3.1 Light-Curing and Ultraviolet-Curing Agents

The exposure of light or UV is used to cure resin and decomposes epoxy resin by the
stability of light- or UV-curing agents. The main advantage of these agents is they
are non-polluting paints and printing inks. The liquid with no solvent is added to
cause the agents to dissolve.
2.4.3.2 Boron Trifluoride–Amine Complex

Boron trifluoride (BF3 ) is a well-known catalyst for several chemical reactions. Leep-
oxy’s LEECURE B series of epoxy curatives is a family of boron trifluoride-based
accelerators. These accelerators span a broad reactivity range and are useful in the
formulation of epoxy systems [26, 27]. Figure 2.14 shows the chemical structure of
boron trifluoride–amine complex.
2.4.3.3 Dicyandiamide
Dicyandiamide (also referred to as DICY) is an alkaline and water-soluble crystalline
compound that is scientifically known as cyanoguanidine. The chemical consists
of two identical cyanamide or cyanoguanidine molecules mixed together, that is
generally used in the making of melamine. Melamine is typically produced by this
method. Laminates for powder coatings, adhesives, and a curing agent for epoxy
resins are some of the many uses of PICY. It can dissolve in diethyl ether, water, and
alcohol. The carbide method is used to prepare it commercially from the carbonate
gotten from limestone or through the desulfurization of thiourea when a catalyst is
introduced (mercuric oxide). Cyanamide can also be prepared by the interaction of
ammonia with cyanogene halides. Cyanamide polymerizes to dicyandiamide (DCY)
when it is heated to a temperature over 150 ∘ C and to tricyantriamide or to melamine
[28, 29]. Figure 2.15 shows the chemical structure of DCY.
2.4.3.4 Organic-Acid Hydrazide

Hydrazides are a category of organic compounds distinguished by a nitrogen to
nitrogen covalent bond made up of four substituents with a minimum of one
NH Figure 2.15 Chemical structure of dicyandiamide.

Source: Yue et al. [29].
N
NH2 NH
NH3HN CO R CO NH3HN
Figure 2.16 Chemical structure of organic acid hydrazide.
being an acyl group. The making of new hydrazide spin-offs is inspired by the
hydrazine group of compounds that have antioxidant, analgesic, anticonvul-
sant, hormone antagonist, antiplatelet, antiviral, vasodilator, antitrypanosomal,
anti-inflammatory, antimalarial, antimycobacterial, antimicrobial, and antitumor
properties [30]. Figure 2.16 shows the chemical structure of organic acid hydrazide.
2.4.4 Curing Conditions

2.4.4.1 Bisphenol-A Epoxy Resin
This type of epoxy resin cures at room temperature which is scientifically considered
to be 20–25 ∘ C and also under heated conditions [31, 32].
2.4.4.2 Bisphenol-F Epoxy Resin

This type of epoxy resin cures at room temperature and also under heat conditions
[31, 32].
2.4.4.3 Phenol Novolac Epoxy Resin

This type of epoxy resin cures at room temperature and also under heat conditions
[31, 32].
2.4.4.4 Cycloaliphatic Epoxy Resin

This type of epoxy resin cures under UV light and under heat conditions [31].
2.4.4.5 Glycidylamine Epoxy Resin

Though some epoxy/hardener mixtures curate at room temperature (i.e. the air
temperature of the environment), glycidylamine resin needs heat to cure. Com-
monly, temperatures reaching 150 ∘ C are used but some special set-ups will use
up to 200 ∘ C. If not enough heat is added during the curing process, incomplete
polymerization will occur which will result in reduced mechanical, chemical, and
heat resistance [33].
2.5 Reaction Mechanisms

2.5.1 Bisphenol-A Epoxy Resin
Curing reaction of this type of resin based on the experiment that was conducted
indicated that the structure was profound when a ratio of 10 : 3 of bisphenol-A
2.5 Reaction Mechanisms 35
epoxy resin (DER331) to the curing agent (DEH622) and the reactional heat was
358.53 J/g which is four times to nine greater than the heat released by other
different ratios. The minimum curing temperature was 36.35 ∘ C which is lesser
than the other different ratios; maximum curing temperature was 10–40 ∘ C lower
than other proportion [34].
2.5.2 Bisphenol-F Epoxy Resin

This type of resin undergoes a similar epoxy resin formation as bisphenol-A. By
observation from these resins, the mean epoxy content is higher with lower viscos-
ity per gram than bisphenol-A category of resins, which increases their chemical
resistance [14].
If it is synthesized from phenol formaldehyde and epichlorohydrin, oxalic acid is
used as a catalyst. Commonly, resin had epoxide number of 0.65–0.68 mol/100 g and
viscosity of 1.3 Pa s [35].
2.5.3 Phenol Novolac Epoxy Resin

By combination of formaldehyde and phenols with subsequent epichlorohydrin, gly-
cidylation results in epoxidised novolacs. This includes EPN and ECN which in
many instances are highly viscous to solid resins, generally has same mean epox-
ide functionality of around two to six. A polymer network that is highly cross-linked
can be formed showing high chemical resistance and temperature from the high
epoxide functionality of these resins.This however has low flexibility [14].
Epoxy novolac resins are described as multifunctional epoxy resins because it has
two or more epoxy groups per molecule; by chemical reacting a phenolic novolac
resin with epichlorohydrin, polyepoxides are obtained. Upon processing, a high
cross-link density can be achieved because of the increased functionality in epoxies.
This is generally recommended for appliactions requiring high performance
which in turn require the best resistence to chemical, resistance to solvents, and
outstanding temperature in high application resistance compared to the standard
bisphenol-A epoxy. Epoxy novolac resins in most instances can also be applied
in blend formulas to upgrade the performance produced by bisphenol-A and
bisphenol-F epoxy resins [36].
2.5.4 Cycloaliphatic Epoxy Resin

Glycidyl ethers are base reactive and are principally reactive with polyamine
hardener, while acidic hardeners, such as anhydrides of dibasic acids, cause
cycloaliphatic epoxides. Recently, a vast variety of studies on different kind of
catalysts called the latent catalysts which can produce reactive species to initiate
polymerization by suitable stimulation, e.g. over irradiation or heating, were carried
out [37].
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comme bon lui semble, mais je ne les lui prête que sur la promesse
qu’elle m’a faite de souscrire un contrat avec lequel je puisse
prendre mes sûretés sur sa part dans les terrains nus de Waignies.
Marguerite détourna la tête pour ne pas laisser voir les larmes
qui lui vinrent aux yeux, elle connaissait la pureté de cœur qui
distinguait Emmanuel. Élevé par son oncle dans la pratique la plus
sévère des vertus religieuses, le jeune homme avait spécialement
horreur du mensonge; après avoir offert sa vie et son cœur à
Marguerite, il lui faisait donc encore le sacrifice de sa conscience.
—Adieu, monsieur, lui dit Balthazar, je vous croyais plus de
confiance dans un homme qui vous voyait avec des yeux de père.
Après avoir échangé avec Marguerite un déplorable regard,
Emmanuel fut reconduit par Martha qui ferma la porte de la rue. Au
moment où le père et la fille furent bien seuls, Claës dit à sa fille:—
Tu m’aimes, n’est-ce pas?
—Ne prenez pas de détours, mon père. Vous voulez cette
somme, vous ne l’aurez point.
Elle se mit à rassembler les ducats, son père l’aida
silencieusement à les ramasser et à vérifier la somme qu’elle avait
semée, et Marguerite le laissa faire sans lui témoigner la moindre
défiance. Les deux milles ducats remis en pile, Balthazar dit d’un air
désespéré:—Marguerite, il me faut cet or!
—Ce serait un vol si vous le preniez, répondit-elle froidement.
Écoutez, mon père: il vaut mieux nous tuer d’un seul coup, que de
nous faire souffrir mille morts chaque jour. Voyez, qui de vous, qui de
nous doit succomber.
—Vous aurez donc assassiné votre père, reprit-il.
—Nous aurons vengé notre mère, dit-elle en montrant la place où
madame Claës était morte.
—Ma fille, si tu savais ce dont il s’agit, tu ne me dirais pas de
telles paroles. Écoute, je vais t’expliquer le problème... Mais tu ne
me comprendras pas? s’écria-t-il avec désespoir. Enfin, donne! crois
une fois en ton père. Oui, je sais que j’ai fait de la peine à ta mère;
que j’ai dissipé, pour employer le mot des ignorants, ma fortune et
dilapidé la vôtre; que vous travaillez tous pour ce que tu nommes
une folie; mais, mon ange, ma bien-aimée, mon amour, ma
Marguerite, écoute-moi donc! Si je ne réussis pas, je me donne à toi,
je t’obéirai comme tu devrais, toi, m’obéir; je ferai tes volontés, je te
remettrai la conduite de ma fortune, je ne serai plus le tuteur de mes
enfants, je me dépouillerai de toute autorité. Je le jure par ta mère,
dit-il en versant des larmes. Marguerite détourna la tête pour ne pas
voir cette figure en pleurs, et Claës se jeta aux genoux de sa fille en
croyant qu’elle allait céder.—Marguerite, Marguerite! donne, donne!
Que sont soixante mille francs pour éviter des remords éternels!
Vois-tu, je mourrai, ceci me tuera. Écoute-moi! ma parole sera
sacrée. Si j’échoue, je renonce à mes travaux, je quitterai la Flandre,
la France même, si tu l’exiges, et j’irai travailler comme un
manœuvre afin de refaire sou à sou ma fortune et rapporter un jour à
mes enfants ce que la Science leur aura pris. Marguerite voulait
relever son père, mais il persistait à rester à ses genoux, et il ajouta
en pleurant:—Sois une dernière fois, tendre et dévouée? Si je ne
réussis pas, je te donnerai moi-même raison dans tes duretés. Tu
m’appelleras vieux fou! tu me nommeras mauvais père! enfin tu me
diras que je suis un ignorant! Moi, quand j’entendrai ces paroles, je
te baiserai les mains. Tu pourras me battre, si tu le veux; et quand tu
me frapperas, je te bénirai comme la meilleure des filles en me
souvenant que tu m’as donné ton sang!
—S’il ne s’agissait que de mon sang, je vous le rendrais, s’écria-
t-elle, mais puis-je laisser égorger par la Science mon frère et ma
sœur? non! Cessez, cessez, dit-elle en essuyant ses larmes et
repoussant les mains caressantes de son père.
—Soixante-mille francs et deux mois, dit-il en se levant avec
rage, il ne me faut plus que cela; mais ma fille se met entre la gloire,
entre la richesse et moi. Sois maudite! ajouta-t-il. Tu n’es ni fille, ni
femme, tu n’as pas de cœur, tu ne seras ni une mère, ni une
épouse, ajouta-t-il. Laisse-moi prendre! dis, ma chère petite, mon
enfant chérie, je t’adorerai, ajouta-t-il en avançant la main sur l’or par
un mouvement d’atroce énergie.
—Je suis sans défense contre la force, mais Dieu et le grand
Claës nous voient! dit Marguerite en montrant le portrait.
—Eh! bien, essaie de vivre couverte du sang de ton père, cria
Balthazar en lui jetant un regard d’horreur. Il se leva, contempla le
parloir et sortit lentement. En arrivant à la porte, il se retourna
comme eût fait un mendiant et interrogea sa fille par un geste auquel
Marguerite répondit en faisant un signe de tête négatif.—Adieu, ma
fille, dit-il avec douceur, tâchez de vivre heureuse.
Quand il eut disparu, Marguerite resta dans une stupeur qui eut
pour effet de l’isoler de la terre, elle n’était plus dans le parloir, elle
ne sentait plus son corps, elle avait des ailes, et volait dans les
espaces du monde moral où tout est immense, où la pensée
rapproche et les distances et les temps, où quelque main divine
relève la toile étendue sur l’avenir. Il lui sembla qu’il s’écoulait des
jours entiers entre chacun des pas que faisait son père en montant
l’escalier; puis elle eut un frisson d’horreur au moment où elle
l’entendit entrer dans sa chambre. Guidée par un pressentiment qui
répandit dans son âme la poignante clarté d’un éclair, elle franchit
les escaliers sans lumière, sans bruit, avec la vélocité d’une flèche,
et vit son père qui s’ajustait le front avec un pistolet.
—Prenez tout, lui cria-t-elle en s’élançant vers lui.
Elle tomba sur un fauteuil. Balthazar la voyant pâle, se mit à
pleurer comme pleurent les vieillards; il redevint enfant, il la baisa au
front, lui dit des paroles sans suite, il était près de sauter de joie, et
semblait vouloir jouer avec elle comme un amant joue avec sa
maîtresse après en avoir obtenu le bonheur.
—Assez! assez, mon père, dit-elle, songez à votre promesse! Si
vous ne réussissez pas, vous m’obéirez!
—Oui.
—O ma mère, dit-elle en se tournant vers la chambre de
madame Claës, vous auriez tout donné, n’est-ce pas?
—Dors en paix, dit Balthazar, tu es une bonne fille.
—Dormir! dit-elle, je n’ai plus les nuits de ma jeunesse; vous me
vieillissez, mon père, comme vous avez lentement flétri le cœur de
ma mère.
—Pauvre enfant, je voudrais te rassurer en t’expliquant les effets
de la magnifique expérience que je viens d’imaginer, tu
comprendrais.
—Je ne comprends que notre ruine, dit-elle en s’en allant.
Le lendemain matin, qui était un jour de congé, Emmanuel de
Solis amena Jean.
—Hé bien? dit-il avec tristesse en abordant Marguerite.
—J’ai cédé, répondit-elle.
—Ma chère vie, dit-il avec un mouvement de joie mélancolique,
si vous aviez résisté, je vous eusse admirée; mais faible, je vous
adore!
—Pauvre, pauvre Emmanuel, que nous restera-t-il?
—Laissez-moi faire, s’écria le jeune homme d’un air radieux,
nous nous aimons, tout ira bien!
Quelques mois s’écoulèrent dans une tranquillité parfaite.
Monsieur de Solis fit comprendre à Marguerite que ses chétives
économies ne constitueraient jamais une fortune, et lui conseilla de
vivre à l’aise en prenant, pour maintenir l’abondance au logis,
l’argent qui restait sur la somme de laquelle il avait été le
dépositaire. Pendant ce temps, Marguerite fut livrée aux anxiétés qui
jadis avaient agité sa mère en semblable occurrence. Quelque
incrédule qu’elle pût être, elle en était arrivée à espérer dans le
génie de son père. Par un phénomène inexplicable, beaucoup de
gens ont l’espérance sans avoir la foi. L’espérance est la fleur du
Désir, la foi est le fruit de la Certitude. Marguerite se disait: «Si mon
père réussit, nous serons heureux!» Claës et Lemulquinier seuls
disaient: «Nous réussirons!» Malheureusement, de jour en jour, le
visage de cet homme s’attrista. Quand il venait dîner, il n’osait
parfois regarder sa fille et parfois il lui jetait aussi des regards de
triomphe. Marguerite employa ses soirées à se faire expliquer par le
jeune de Solis plusieurs difficultés légales. Elle accabla son père de
questions sur leurs relations de famille. Enfin elle acheva son
éducation virile, elle se préparait évidemment à exécuter le plan
qu’elle méditait si son père succombait encore une fois dans son
duel avec l’Inconnu (X).
Au commencement du mois de juillet, Balthazar passa toute une
journée assis sur le banc de son jardin, plongé dans une méditation
triste. Il regarda plusieurs fois le tertre dénué de tulipes, les fenêtres
de la chambre de sa femme; il frémissait sans doute en songeant à
tout ce que sa lutte lui avait coûté: ses mouvements attestaient des
pensées en dehors de la Science. Marguerite vint s’asseoir et
travailler près de lui quelques moments avant le dîner.
—Hé! bien, mon père, vous n’avez pas réussi.
—Non, mon enfant.
—Ah! dit Marguerite d’une voix douce, je ne vous adresserai pas
le plus léger reproche, nous sommes également coupables. Je
réclamerai seulement l’exécution de votre parole, elle doit être
sacrée, vous êtes un Claës. Vos enfants vous entoureront d’amour
et de respect; mais d’aujourd’hui vous m’appartenez, et me devez
obéissance. Soyez sans inquiétude, mon règne sera doux, et je
travaillerai même à le faire promptement finir. J’emmène Martha, je
vous quitte pour un mois environ, et pour m’occuper de vous, car,
dit-elle en le baisant au front, vous êtes mon enfant. Demain, Félicie
conduira donc la maison. La pauvre enfant n’a que dix-sept ans, elle
ne saurait pas vous résister; soyez généreux, ne lui demandez pas
un sou, car elle n’aura que ce qu’il lui faut strictement pour les
dépenses de la maison. Ayez du courage, renoncez pendant deux
ou trois années à vos travaux et à vos pensées. Le problème mûrira,
je vous aurai amassé l’argent nécessaire pour le résoudre et vous le
résoudrez. Hé! bien, votre reine n’est-elle pas clémente, dites?
—Tout n’est donc pas perdu, dit le vieillard.
—Non, si vous êtes fidèle à votre parole.
—Je vous obéirai, ma fille, répondit Claës avec une émotion
profonde.
Le lendemain, monsieur Conyncks de Cambrai vint chercher sa
petite nièce. Il était en voiture de voyage, et ne voulut rester chez
son cousin que le temps nécessaire à Marguerite et à Martha pour
faire leurs apprêts. Monsieur Claës reçut son cousin avec affabilité,
mais il était visiblement triste et humilié. Le vieux Conyncks devina
les pensées de Balthazar, et, en déjeunant, il lui dit avec une grosse
franchise:—J’ai quelques-uns de vos tableaux, cousin, j’ai le goût
des beaux tableaux, c’est une passion ruineuse; mais, nous avons
tous notre folie...
—Cher oncle! dit Marguerite.
—Vous passez pour être ruiné, cousin, mais un Claës a toujours
des trésors là, dit-il en se frappant le front. Et là, n’est-ce pas?
ajouta-t-il en montrant son cœur. Aussi compté-je sur vous! J’ai
trouvé dans mon escarcelle quelques écus que j’ai mis à votre
service.
—Ha! s’écria Balthazar, je vous rendrai des trésors...
—Les seuls trésors que nous possédions en Flandre, cousin,
c’est la patience et le travail, répondit sévèrement Conyncks. Notre
ancien a ces deux mots gravés sur le front, dit-il en lui montrant le
portrait du président Van-Claës.
Marguerite embrassa son père, lui dit adieu, fit ses
recommandations à Josette, à Félicie, et partit en poste pour Paris.
Le grand-oncle devenu veuf n’avait qu’une fille de douze ans et
possédait une immense fortune, il n’était donc pas impossible qu’il
voulût se marier; aussi les habitants de Douai crurent-ils que
mademoiselle Claës épousait son grand-oncle. Le bruit de ce riche
mariage ramena Pierquin le notaire chez les Claës. Il s’était fait de
grands changements dans les idées de cet excellent calculateur.
Depuis deux ans, la société de la ville s’était divisée en deux camps
ennemis. La noblesse avait formé un premier cercle, et la
bourgeoisie un second, naturellement fort hostile au premier. Cette
séparation subite qui eut lieu dans toute la France et la partagea en
deux nations ennemies, dont les irritations jalouses allèrent en
croissant, fut une des principales raisons qui firent adopter la
révolution de juillet 1830 en province. Entre ces deux sociétés, dont
l’une était ultra-monarchique et l’autre ultra-libérale, se trouvaient les
fonctionnaires admis, suivant leur importance, dans l’un et dans
l’autre monde, et qui, au moment de la chute du pouvoir légitime,
furent neutres. Au commencement de la lutte entre la noblesse et la
bourgeoisie, les Cafés royalistes contractèrent une splendeur inouïe,
et rivalisèrent si brillamment avec les Cafés libéraux, que ces sortes
de fêtes gastronomiques coûtèrent, dit-on, la vie à plusieurs
personnages qui, semblables à des mortiers mal fondus, ne purent
résister à ces exercices. Naturellement, les deux sociétés devinrent
exclusives et s’épurèrent. Quoique fort riche pour un homme de
province, Pierquin fut exclu des cercles aristocratiques, et refoulé
dans ceux de la bourgeoisie. Son amour-propre eut beaucoup à
souffrir des échecs successifs qu’il reçut en se voyant
insensiblement éconduit par les gens avec lesquels il frayait
naguère. Il atteignait l’âge de quarante ans, seule époque de la vie
où les hommes qui se destinent au mariage puissent encore
épouser des personnes jeunes. Les partis auxquels il pouvait
prétendre appartenaient à la bourgeoisie, et son ambition tendait à
rester dans le haut monde, où devait l’introduire une belle alliance.
L’isolement dans lequel vivait la famille Claës l’avait rendue
étrangère à ce mouvement social. Quoique Claës appartînt à la
vieille aristocratie de la province, il était vraisemblable que ses
préoccupations l’empêcheraient d’obéir aux antipathies créées par
ce nouveau classement de personnes. Quelque pauvre qu’elle pût
être, une demoiselle Claës apportait à son mari cette fortune de
vanité que souhaitent tous les parvenus. Pierquin revint donc chez
les Claës avec une secrète intention de faire les sacrifices
nécessaires pour arriver à la conclusion d’un mariage qui réalisait
désormais toutes ses ambitions. Il tint compagnie à Balthazar et à
Félicie pendant l’absence de Marguerite, mais il reconnut
tardivement un concurrent redoutable dans Emmanuel de Solis. La
succession du défunt abbé passait pour être considérable; et, aux
yeux d’un homme qui chiffrait naïvement toutes les choses de la vie,
le jeune héritier paraissait plus puissant par son argent que par les
séductions du cœur dont ne s’inquiétait jamais Pierquin. Cette
fortune rendait au nom de Solis toute sa valeur. L’or et la noblesse
étaient comme deux lustres qui, s’éclairant l’un par l’autre,
redoublaient d’éclat. L’affection sincère que le jeune proviseur
témoignait à Félicie, qu’il traitait comme une sœur, excita l’émulation
du notaire. Il essaya d’éclipser Emmanuel en mêlant le jargon à la
mode et les expressions d’une galanterie superficielle aux airs
rêveurs, aux élégies soucieuses qui allaient si bien à sa
physionomie. En se disant désenchanté de tout au monde, il tournait
les yeux vers Félicie de manière à lui faire croire qu’elle seule
pourrait le réconcilier avec la vie. Félicie, à qui pour la première fois
un homme adressait des compliments, écouta ce langage toujours si
doux, même quand il est mensonger; elle prit le vide pour de la
profondeur, et, dans le besoin qui l’oppressait de fixer les sentiments
vagues dont surabondait son cœur, elle s’occupa de son cousin.
Jalouse, à son insu peut-être, des attentions amoureuses
qu’Emmanuel prodiguait à sa sœur, elle voulait sans doute se voir,
comme elle, l’objet des regards, des pensées et des soins d’un
homme. Pierquin démêla facilement la préférence que Félicie lui
accordait sur Emmanuel, et ce fut pour lui une raison de persister
dans ses efforts, en sorte qu’il s’engagea plus qu’il ne le voulait.
Emmanuel surveilla les commencements de cette passion fausse
peut-être chez le notaire, naïve chez Félicie dont l’avenir était en jeu.
Il s’ensuivit, entre la cousine et le cousin, quelques causeries
douces, quelques mots dits à voix basse en arrière d’Emmanuel,
enfin de ces petites tromperies qui donnent à un regard, à une
parole une expression dont la douceur insidieuse peut causer
d’innocentes erreurs. A la faveur du commerce que Pierquin
entretenait avec Félicie, il essaya de pénétrer le secret du voyage
entrepris par Marguerite, afin de savoir s’il s’agissait de mariage et
s’il devait renoncer à ses espérances; mais, malgré sa grosse
finesse, ni Balthazar ni Félicie ne purent lui donner aucune lumière,
par la raison qu’ils ne savaient rien des projets de Marguerite qui, en
prenant le pouvoir, semblait en avoir suivi les maximes en taisant
ses projets. La morne tristesse de Balthazar et son affaissement
rendaient les soirées difficiles à passer. Quoique Emmanuel eût
réussi à faire jouer le chimiste au trictrac, Balthazar y était distrait; et
la plupart du temps cet homme, si grand par son intelligence,
semblait stupide. Déchu de ses espérances, humilié d’avoir dévoré
trois fortunes, joueur sans argent, il pliait sous le poids de ses
ruines, sous le fardeau de ses espérances moins détruites que
trompées. Cet homme de génie, muselé par la nécessité, se
condamnant lui-même, offrait un spectacle vraiment tragique qui eût
touché l’homme le plus insensible. Pierquin lui-même ne contemplait
pas sans un sentiment de respect ce lion en cage, dont les yeux
pleins d’une puissance refoulée étaient devenus calmes à force de
tristesse, ternes à force de lumière; dont les regards demandaient
une aumône que la bouche n’osait proférer. Parfois un éclair passait
sur cette face desséchée qui se ranimait par la conception d’une
nouvelle expérience; puis, si, en contemplant le parloir, les yeux de
Balthazar s’arrêtaient à la place où sa femme avait expiré, de légers
pleurs roulaient comme d’ardents grains de sable dans le désert de
ses prunelles que la pensée faisait immenses, et sa tête retombait
sur sa poitrine. Il avait soulevé le monde comme un Titan, et le
monde revenait plus pesant sur sa poitrine. Cette gigantesque
douleur, si virilement contenue, agissait sur Pierquin et sur
Emmanuel qui, parfois, se sentaient assez émus pour vouloir offrir à
cet homme la somme nécessaire à quelque série d’expériences; tant
sont communicatives les convictions du génie! Tous deux
concevaient comment madame Claës et Marguerite avaient pu jeter
des millions dans ce gouffre: mais la raison arrêtait promptement les
élans du cœur; et leurs émotions se traduisaient par des
consolations qui aigrissaient encore les peines de ce Titan foudroyé.
Claës ne parlait point de sa fille aînée, et ne s’inquiétait ni de son
absence, ni du silence qu’elle gardait en n’écrivant ni à lui, ni à
Félicie. Quand Solis et Pierquin lui en demandaient des nouvelles, il
paraissait affecté désagréablement. Pressentait-il que Marguerite
agissait contre lui? Se trouvait-il humilié d’avoir résigné les droits
majestueux de la paternité à son enfant? En était-il venu à moins
l’aimer parce qu’elle allait être le père, et lui l’enfant? Peut-être y
avait-il beaucoup de ces raisons et beaucoup de ces sentiments
inexprimables qui passent comme des nuages en l’âme, dans la
disgrâce muette qu’il faisait peser sur Marguerite. Quelque grands
que puissent être les grands hommes connus ou inconnus, heureux
ou malheureux dans leurs tentatives, ils ont des petitesses par
lesquelles ils tiennent à l’humanité. Par un double malheur, il ne
souffrent pas moins de leurs qualités que de leurs défauts; et peut-
être Balthazar avait-il à se familiariser avec les douleurs de ses
vanités blessées. La vie qu’il menait, et les soirées pendant
lesquelles ces quatre personnes se trouvèrent réunies en l’absence
de Marguerite furent donc une vie et des soirées empreintes de
tristesse, remplies d’appréhensions vagues. Ce fut des jours
infertiles comme des landes desséchées, où néanmoins ils glanaient
quelques fleurs, rares consolations. L’atmosphère leur semblait
brumeuse en l’absence de la fille aînée, devenue l’âme, l’espoir et la
force de cette famille. Deux mois se passèrent ainsi, pendant
lesquels Balthazar attendit patiemment sa fille. Marguerite fut
ramenée à Douai par son oncle, qui resta au logis au lieu de
retourner à Cambrai, sans doute pour y appuyer de son autorité
quelque coup d’état médité par sa nièce. Ce fut une petite fête de
famille que le retour de Marguerite. Le notaire et monsieur de Solis
avaient été invités à dîner par Félicie et par Balthazar. Quand la
voiture de voyage s’arrêta devant la porte de la maison, ces quatre
personnes vinrent y recevoir les voyageurs avec de grandes
démonstrations de joie. Marguerite parut heureuse de revoir les
foyers paternels, ses yeux s’emplirent de larmes quand elle traversa
la cour pour arriver au parloir. En embrassant son père, ses
caresses de jeune fille ne furent pas néanmoins sans arrière-
pensée, elle rougissait comme une épouse coupable qui ne sait pas
feindre; mais ses regards reprirent leur pureté quand elle regarda
monsieur de Solis, en qui elle semblait puiser la force d’achever
l’entreprise qu’elle avait secrètement formée. Pendant le dîner,
malgré l’allégresse qui animait les physionomies et les paroles, le
père et la fille s’examinèrent avec défiance et curiosité. Balthazar ne
fit à Marguerite aucune question sur son séjour à Paris, sans doute
par dignité paternelle. Emmanuel de Solis imita cette réserve. Mais
Pierquin, qui était habitué à connaître tous les secrets de famille, dit
à Marguerite en couvrant sa curiosité sous une fausse bonhomie:—
Eh! bien, chère cousine, vous avez vu Paris, les spectacles...
—Je n’ai rien vu à Paris, répondit-elle, je n’y suis pas allée pour
me divertir. Les jours s’y sont tristement écoulés pour moi, j’étais
trop impatiente de revoir Douai.
—Si je ne m’étais pas fâché, elle ne serait pas venue à l’Opéra,
où d’ailleurs elle s’est ennuyée! dit monsieur Conyncks.
La soirée fut pénible, chacun était gêné, souriait mal ou
s’efforçait de témoigner cette gaieté de commande sous laquelle se
cachent de réelles anxiétés. Marguerite et Balthazar étaient en proie
à de sourdes et cruelles appréhensions qui réagissaient sur les
cœurs. Plus la soirée s’avançait, plus la contenance du père et de la
fille s’altérait. Parfois Marguerite essayait de sourire, mais ses
gestes, ses regards, le son de sa voix trahissaient une vive
inquiétude. Messieurs Conyncks et de Solis semblaient connaître la
cause des secrets mouvements qui agitaient cette noble fille, et
paraissaient l’encourager par des œillades expressives. Blessé
d’avoir été mis en dehors d’une résolution et de démarches
accomplies pour lui, Balthazar se séparait insensiblement de ses
enfants et de ses amis, en affectant de garder le silence. Marguerite
allait sans doute lui découvrir ce qu’elle avait décidé de lui. Pour un
homme grand, pour un père, cette situation était intolérable. Parvenu
à un âge où l’on ne dissimule rien au milieu de ses enfants, où
l’étendue des idées donne de la force aux sentiments, il devenait
donc de plus en plus grave, songeur et chagrin, en voyant
s’approcher le moment de sa mort civile. Cette soirée renfermait une
de ces crises de la vie intérieure qui ne peuvent s’expliquer que par
des images. Les nuages et la foudre s’amoncelaient au ciel, l’on riait
dans la campagne; chacun avait chaud, sentait l’orage, levait la tête
et continuait sa route. Monsieur Conyncks, le premier, alla se
coucher et fut conduit à sa chambre par Balthazar. Pendant son
absence, Pierquin et monsieur de Solis s’en allèrent. Marguerite fit
un adieu plein d’affection au notaire, elle ne dit rien à Emmanuel,
mais elle lui pressa la main en lui jetant un regard humide. Elle
renvoya Félicie, et quand Claës revint au parloir, il y trouva sa fille
seule.
—Mon bon père, lui dit-elle d’une voix tremblante, il a fallu les
circonstances graves où nous sommes pour me faire quitter la
maison; mais, après bien des angoisses et après avoir surmonté des
difficultés inouïes, j’y reviens avec quelques chances de salut pour
nous tous. Grâce à votre nom, à l’influence de notre oncle et aux
protections de monsieur de Solis, nous avons obtenu, pour vous,
une place de receveur des finances en Bretagne; elle vaut, dit-on,
dix-huit à vingt mille francs par an. Notre oncle a fait le
cautionnement. Voici votre nomination, dit-elle en tirant une lettre de
son sac. Votre séjour ici, pendant nos années de privations et de
sacrifices, serait intolérable. Notre père doit rester dans une situation
au moins égale à celle où il a toujours vécu. Je ne vous demanderai
rien sur vos revenus, vous les emploierez comme bon vous
semblera. Je vous supplie seulement de songer que nous n’avons
pas un sou de rente, et que nous vivrons tous avec ce que Gabriel
nous donnera sur ses revenus. La ville ne saura rien de cette vie
claustrale. Si vous étiez chez vous, vous seriez un obstacle aux
moyens que nous emploierons, ma sœur et moi, pour tâcher d’y
rétablir l’aisance. Est-ce abuser de l’autorité que vous m’avez
donnée que de vous mettre dans une position à refaire vous-même
votre fortune? dans quelques années, si vous le voulez, vous serez
Receveur-général.
—Ainsi, Marguerite, dit doucement Balthazar, tu me chasses de
ma maison.
—Je ne mérite pas un reproche si dur, répondit la fille en
comprimant les mouvements tumultueux de son cœur. Vous
reviendrez parmi nous lorsque vous pourrez habiter votre ville natale
comme il vous convient d’y paraître. D’ailleurs, mon père, n’ai-je
point votre parole? reprit-elle froidement. Vous devez m’obéir. Mon
oncle est resté pour vous emmener en Bretagne, afin que vous ne
fissiez pas seul le voyage.
—Je n’irai pas, s’écria Balthazar en se levant, je n’ai besoin du
secours de personne pour rétablir ma fortune et payer ce que je dois
à mes enfants.
—Ce sera mieux, reprit Marguerite sans s’émouvoir. Je vous
prierai de réfléchir à notre situation respective que je vais vous
expliquer en peu de mots. Si vous restez dans cette maison, vos
enfants en sortiront, afin de vous en laisser le maître.
—Marguerite! cria Balthazar.
—Puis, dit-elle en continuant sans vouloir remarquer l’irritation de
son père, il faut instruire le ministre de votre refus, si vous
n’acceptez pas une place lucrative et honorable que, malgré nos
démarches et nos protections, nous n’aurions pas eue sans
quelques billets de mille francs adroitement mis par mon oncle dans
le gant d’une dame.
—Me quitter!
—Ou vous nous quitterez ou nous vous fuirons, dit-elle. Si j’étais
votre seule enfant, j’imiterais ma mère, sans murmurer contre le sort
que vous me feriez. Mais ma sœur et mes deux frères ne périront
pas de faim ou de désespoir auprès de vous; je l’ai promis à celle
qui mourut là, dit-elle en montrant la place du lit de sa mère. Nous
vous avons caché nos douleurs, nous avons souffert en silence,
aujourd’hui nos forces se sont usées. Nous ne sommes pas au bord
d’un abîme, nous sommes au fond, mon père! pour nous en tirer, il
ne nous faut pas seulement du courage, il faut encore que nos
efforts ne soient pas incessamment déjoués par les caprices d’une
passion...
—Mes chers enfants! s’écria Balthazar, en saisissant la main de
Marguerite, je vous aiderai, je travaillerai, je...
—En voici les moyens, répondit-elle en lui tendant la lettre
ministérielle.
—Mais, mon ange, le moyen que tu m’offres pour refaire ma
fortune est trop lent! tu me fais perdre le fruit de dix années de
travaux, et les sommes énormes que représente mon laboratoire.
Là, dit-il en indiquant le grenier, sont toutes nos ressources.
Marguerite marcha vers la porte en disant:—Mon père, vous
choisirez!
—Ah! ma fille, vous êtes bien dure! répondit-il en s’asseyant dans
un fauteuil et la laissant partir.
Le lendemain matin, Marguerite apprit par Lemulquinier que
monsieur Claës était sorti. Cette simple annonce la fit pâlir, et sa
contenance fut si cruellement significative, que le vieux valet lui dit:
—Soyez tranquille, mademoiselle, monsieur a dit qu’il serait revenu
à onze heures pour déjeuner. Il ne s’est pas couché. A deux heures
du matin, il était encore debout dans le parloir, à regarder par les
fenêtres les toits du laboratoire. J’attendais dans la cuisine, je le
voyais, il pleurait, il a du chagrin. Voici ce fameux mois de juillet
pendant lequel le soleil est capable de nous enrichir tous, et si vous
vouliez...
—Assez! dit Marguerite en devinant toutes les pensées qui
avaient dû assaillir son père.
Il s’était en effet accompli chez Balthazar ce phénomène qui
s’empare de toutes les personnes sédentaires, sa vie dépendait
pour ainsi dire des lieux avec lesquels il s’était identifié, sa pensée
mariée à son laboratoire et à sa maison les lui rendait
indispensables, comme l’est la Bourse au joueur pour qui les jours
fériés sont des jours perdus. Là étaient ses espérances, là
descendait du ciel la seule atmosphère où ses poumons pouvaient
puiser l’air vital. Cette alliance des lieux et des choses entre les
hommes, si puissante chez les natures faibles, devient presque
tyrannique chez les gens de science et d’étude. Quitter sa maison,
c’était, pour Balthazar, renoncer à la Science, à son problème, c’était
mourir. Marguerite fut en proie à une extrême agitation jusqu’au
moment du déjeuner. La scène qui avait porté Balthazar à vouloir se
tuer lui était revenue à la mémoire, et elle craignit de voir se dénouer
tragiquement la situation désespérée où se trouvait son père. Elle
allait et venait dans le parloir, en tressaillant chaque fois que la
sonnette de la porte retentissait. Enfin, Balthazar revint. Pendant
qu’il traversait la cour, Marguerite, qui étudia sa figure avec
inquiétude, n’y vit que l’expression d’une douleur orageuse. Quand il
entra dans le parloir, elle s’avança vers lui pour lui souhaiter le
bonjour; il la saisit affectueusement par la taille, l’appuya sur son
cœur, la baisa au front et lui dit à l’oreille:—Je suis allé demander
mon passe-port. Le son de la voix, le regard résigné, le mouvement
de son père, tout écrasa le cœur de la pauvre fille qui détourna la
tête pour ne point laisser voir ses larmes; mais ne pouvant les
réprimer, elle alla dans le jardin, et revint après y avoir pleuré à son
aise. Pendant le déjeuner, Balthazar se montra gai comme un
homme qui avait pris son parti.
—Nous allons donc partir pour la Bretagne, mon oncle, dit-il a
monsieur Conyncks. J’ai toujours eu le désir de voir ce pays-là.
—On y vit à bon marché, répondit le vieil oncle.
—Mon père nous quitte? s’écria Félicie.
Monsieur de Solis entra, il amenait Jean.
—Vous nous le laisserez aujourd’hui, dit Balthazar en mettant
son fils près de lui, je pars demain, et je veux lui dire adieu.
Emmanuel regarda Marguerite qui baissa la tête. Ce fut une
journée morne, pendant laquelle chacun fut triste, et réprima des
pensées ou des pleurs. Ce n’était pas une absence, mais un exil.
Puis, tous sentaient instinctivement ce qu’il y avait d’humiliant pour
un père à déclarer ainsi publiquement ses désastres en acceptant
une place et en quittant sa famille à l’âge de Balthazar. Lui seul fut
aussi grand que Marguerite était ferme, et parut accepter noblement
cette pénitence des fautes que l’emportement du génie lui avait fait
commettre. Quand la soirée fut passée et que le père et la fille furent
seuls, Balthazar, qui, pendant toute la journée, s’était montré tendre
et affectueux, comme il l’était durant les beaux jours de sa vie
patriarcale, tendit la main à Marguerite, et lui dit avec une sorte de
tendresse mêlée de désespoir:—Es-tu contente de ton père?
—Vous êtes digne de celui-là, répondit Marguerite en lui
montrant le portrait de Van-Claës.
Le lendemain matin, Balthazar suivi de Lemulquinier monta dans
son laboratoire comme pour faire ses adieux aux espérances qu’il
avait caressées et que ses opérations commencées lui
représentaient vivantes. Le maître et le valet se jetèrent un regard
plein de mélancolie en entrant dans le grenier qu’ils allaient quitter
peut-être pour toujours. Balthazar contempla ces machines sur
lesquelles sa pensée avait si longtemps plané, et dont chacune était
liée au souvenir d’une recherche ou d’une expérience. Il ordonna
d’un air triste à Lemulquinier de faire évaporer des gaz ou des
acides dangereux, de séparer des substances qui auraient pu
produire des explosions. Tout en prenant ces soins, il proférait des
regrets amers, comme en exprime un condamné à mort, avant
d’aller à l’échafaud.
—Voici pourtant, dit-il en s’arrêtant devant une capsule dans
laquelle plongeaient les deux fils d’une pile de Volta, une expérience
dont le résultat devrait être attendu. Si elle réussissait, affreuse
pensée! mes enfants ne chasseraient pas de sa maison un père qui
jetterait des diamants à leurs pieds. Voilà une combinaison de
carbone et de soufre, ajouta-t-il en se parlant à lui-même, dans
laquelle le carbone joue le rôle de corps électro-positif; la
cristallisation doit commencer au pôle négatif; et, dans le cas de
décomposition, le carbone s’y porterait cristallisé...
—Ah! ça se ferait comme ça, dit Lemulquinier en contemplant
son maître avec admiration.
—Or, reprit Balthazar après une pause, la combinaison est
soumise à l’influence de cette pile qui peut agir...
—Si monsieur veut, je vais en augmenter l’effet...
—Non, non, il faut la laisser telle qu’elle est. Le repos et le temps
sont des conditions essentielles à la cristallisation...
—Parbleu, faut qu’elle prenne son temps, cette cristallisation,
s’écria le valet de chambre.
—Si la température baisse, le sulfure de carbone se cristallisera,
dit Balthazar en continuant d’exprimer par lambeaux les pensées
indistinctes d’une méditation complète dans son entendement; mais
si l’action de la pile opère dans certaines conditions que j’ignore... Il
faudrait surveiller cela... il est possible... Mais à quoi pensé-je? il ne
s’agit plus de Chimie, mon ami, nous devons aller gérer une recette
en Bretagne.
Claës sortit précipitamment, et descendit pour faire un dernier
déjeuner de famille auquel assistèrent Pierquin et monsieur de Solis.
Balthazar, pressé d’en finir avec son agonie scientifique, dit adieu à
ses enfants et monta en voiture avec son oncle, toute la famille
l’accompagna sur le seuil de la porte. Là, quand Marguerite eut
embrassé son père par une étreinte désespérée, à laquelle il
répondit en lui disant à l’oreille: «Tu es une bonne fille, et je ne t’en
voudrai jamais!» elle franchit la cour, se sauva dans le parloir,
s’agenouilla à la place où sa mère était morte, et fit une ardente
prière à Dieu pour lui demander la force d’accomplir les rudes
travaux de sa nouvelle vie. Elle était déjà fortifiée par une voix
intérieure qui lui avait jeté dans le cœur les applaudissements des
anges et les remercîments de sa mère, quand sa sœur, son frère,
Emmanuel et Pierquin rentrèrent après avoir regardé la calèche
jusqu’à ce qu’ils ne la vissent plus.
—Maintenant, mademoiselle, qu’allez-vous faire? lui dit Pierquin.
—Sauver la maison, répondit-elle avec simplicité. Nous
possédons près de treize cents arpents à Waignies. Mon intention
est de les faire défricher, les partager en trois fermes, construire les
bâtiments nécessaires à leur exploitation, les louer; et je crois qu’en
quelques années, avec beaucoup d’économie et de patience,
chacun de nous, dit-elle en montrant sa sœur et son frère, aura une
ferme de quatre cents et quelques arpents qui pourra valoir, un jour,
près de quinze mille francs de rente. Mon frère Gabriel gardera pour
sa part cette maison et ce qu’il possède sur le Grand-Livre. Puis
nous rendrons un jour à notre père sa fortune dégagée de toute
obligation, en consacrant nos revenus à l’acquittement de ses
dettes.
—Mais, chère cousine, dit le notaire stupéfait de cette entente
des affaires et de la froide raison de Marguerite, il vous faut plus de
deux cent mille francs pour défricher vos terrains, bâtir vos fermes et
acheter des bestiaux. Où prendrez-vous cette somme?
—Là commencent mes embarras, dit-elle en regardant
alternativement le notaire et monsieur de Solis, je n’ose les
demander à mon oncle qui a déjà fait le cautionnement de mon père!
—Vous avez des amis! s’écria Pierquin en voyant tout à coup
que les demoiselles Claës seraient encore des filles de plus de cinq
cent mille francs.
Emmanuel de Solis regarda Marguerite avec attendrissement,
mais, malheureusement pour lui, Pierquin resta notaire au milieu de
son enthousiasme et reprit ainsi:—Moi, je vous les offre, ces deux
cent mille francs!
Emmanuel et Marguerite se consultèrent par un regard qui fut un
trait de lumière pour Pierquin. Félicie rougit excessivement, tant elle
était heureuse de trouver son cousin aussi généreux qu’elle le
souhaitait. Elle regarda sa sœur qui, tout à coup, devina que
pendant l’absence qu’elle avait faite, la pauvre fille s’était laissé
prendre à quelques banales galanteries de Pierquin.
—Vous ne me paierez que cinq pour cent d’intérêt, dit-il. Vous me
rembourserez quand vous voudrez, et vous me donnerez une
hypothèque sur vos terrains. Mais soyez tranquille, vous n’aurez que
les déboursés à payer pour tous vos contrats, je vous trouverai de
bons fermiers, et ferai vos affaires gratuitement afin de vous aider en
bon parent.
Emmanuel fit un signe à Marguerite pour l’engager à refuser;
mais elle était trop occupée à étudier les changements qui
nuançaient la physionomie de sa sœur pour s’en apercevoir. Après
une pause, elle regarda le notaire d’un air ironique et lui dit d’elle-
même, à la grande joie de monsieur de Solis:—Vous êtes un bien
bon parent, je n’attendais pas moins de vous; mais l’intérêt à cinq
pour cent retarderait trop notre libération, j’attendrai la majorité de
mon frère et nous vendrons ses rentes.
Pierquin se mordit les lèvres, Emmanuel se mit à sourire
doucement.
—Félicie, ma chère enfant, reconduis Jean au collége, Martha
t’accompagnera, dit Marguerite en montrant son frère.—Jean, mon
ange, sois bien sage, ne déchire pas tes habits, nous ne sommes
pas assez riches pour te les renouveler aussi souvent que nous le
faisions! Allons, va, mon petit, étudie bien.
Félicie sortit avec son frère.
—Mon cousin, dit Marguerite à Pierquin, et vous, monsieur, dit-
elle à monsieur de Solis, vous êtes sans doute venus voir mon père
pendant mon absence, je vous remercie de ces preuves d’amitié.
Vous ne ferez sans doute pas moins pour deux pauvres filles qui
vont avoir besoin de conseils. Entendons-nous à ce sujet?... Quand
je serai en ville, je vous recevrai toujours avec le plus grand plaisir;
mais quand Félicie sera seule ici avec Josette et Martha, je n’ai pas
besoin de vous dire qu’elle ne doit voir personne, fût-ce un vieil ami,
et le plus dévoué de nos parents. Dans les circonstances où nous
nous trouvons, notre conduite doit être d’une irréprochable sévérité.
Nous voici donc pour long-temps vouées au travail et à la solitude.
Le silence régna pendant quelques instants. Emmanuel, abîmé
dans la contemplation de la tête de Marguerite, semblait muet,
Pierquin ne savait que dire. Le notaire prit congé de sa cousine, en
éprouvant un mouvement de rage contre lui-même: il avait deviné
tout à coup que Marguerite aimait Emmanuel, et qu’il venait de se
conduire en vrai sot.
—Ah! çà, Pierquin, mon ami, se dit-il en s’apostrophant lui-même
dans la rue, un homme qui te dirait que tu es un grand animal aurait
raison. Suis-je bête? J’ai douze mille livres de rente, en dehors de
ma charge, sans compter la succession de mon oncle Des
Racquets, de qui je suis le seul héritier, et qui me doublera ma
fortune un jour ou l’autre (enfin, je ne lui souhaite pas de mourir, il
est économe!)... et j’ai l’infamie de demander des intérêts à
mademoiselle Claës! Je suis sûr qu’à eux deux ils se moquent
maintenant de moi. Je ne dois plus penser à Marguerite! Non. Après
tout, Félicie est une douce et bonne petite créature qui me convient
mieux. Marguerite a un caractère de fer, elle voudrait me dominer, et
elle me dominerait! Allons, montrons-nous généreux, ne soyons pas
tant notaire, je ne peux donc pas secouer ce harnais là? Sac à
papier, je vais me mettre à aimer Félicie, et je ne bouge pas de ce
sentiment-là! Fourche! elle aura une ferme de quatre cent trente
arpents, qui, dans un temps donné, vaudra entre quinze et vingt
mille livres de rente, car les terrains de Waignies sont bons. Que
mon oncle Des Racquets meure, pauvre bonhomme! je vends mon
Étude et je suis un homme de cin-quan-te-mil-le-li-vres de ren-te. Ma
femme est une Claës, je suis allié à des maisons considérables.
Diantre, nous verrons si les Courteville, les Magalhens, les Savaron
de Savarus refuseront de venir chez un Pierquin-Claës-Molina-
Nourho. Je serai maire de Douai, j’aurai la croix, je puis être député,
j’arrive à tout. Ha! ça, Pierquin, mon garçon, tiens-toi là, ne faisons
plus de sottises, d’autant que, ma parole d’honneur, Félicie...
mademoiselle Félicie Van-Claës, elle t’aime.
Quand les deux amants furent seuls, Emmanuel tendit une main
à Marguerite qui ne put s’empêcher d’y mettre sa main droite. Ils se
levèrent par un mouvement unanime en se dirigeant vers leur banc
dans le jardin; mais au milieu du parloir, l’amant ne put résister à sa
joie, et d’une voix que l’émotion rendit tremblante, il dit à Marguerite:
—J’ai trois cent mille francs à vous!...
—Comment, s’écria-t-elle, ma pauvre mère vous aurait encore
confié?... Non. Quoi?
—Oh! ma Marguerite, ce qui est à moi n’est-il pas à vous? N’est-
ce pas vous qui la première avez dit nous?
—Cher Emmanuel, dit-elle en pressant la main qu’elle tenait
toujours; et, au lieu d’aller au jardin, elle se jeta dans la bergère.
—N’est-ce pas à moi de vous remercier, dit-il avec sa voix
d’amour, puisque vous acceptez.
—Ce moment, dit-elle, mon cher bien-aimé, efface bien des
douleurs, et rapproche un heureux avenir! Oui, j’accepte ta fortune,
reprit-elle en laissant errer sur ses lèvres un sourire d’ange, je sais le
moyen de la faire mienne. Elle regarda le portrait de Van-Claës
comme pour avoir un témoin. Le jeune homme qui suivait les
regards de Marguerite ne lui vit pas tirer de son doigt une bague de
jeune fille, et ne s’aperçut de ce geste qu’au moment où il entendit
ces paroles:—Au milieu de nos profondes misères, il surgit un
bonheur. Mon père me laisse, par insouciance, la libre disposition de
moi-même, dit-elle en tendant la bague, prends Emmanuel? Ma
mère te chérissait, elle t’aurait choisi.
Les larmes vinrent aux yeux d’Emmanuel, il pâlit, tomba sur ses
genoux, et dit à Marguerite en lui donnant un anneau qu’il portait
toujours:—Voici l’alliance de ma mère! Ma Marguerite, reprit-il en
baisant la bague, n’aurai-je donc d’autre gage que ceci!
Elle se baissa pour apporter son front aux lèvres d’Emmanuel.

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Epoxy Composites Jyotishkumar

Nanotechnology-Enhanced Food Packaging Jyotishkumar

Encyclopedia of Materials: Composites: Composites.

Explosion blast response of composites Mouritz

Polymer Composites for Electrical Engineering Xingyi

Lignin in Polymer Composites 1st Edition Faruk

Design and Manufacturing of Structural Composites Lee

Green composites for automotive applications Koronis

Multiscale Modeling Approaches for Composites 1st

Fabrication, Characterization and Applications

Cover Image: © Igor Krutov/Alamy Stock Print ISBN: 978-3-527-34678-3

Typesetting SPi Global, Chennai, India

Printed on acid-free paper

1 Introduction to Epoxy Composites 1

2 Synthesis and Manufacturing of Epoxy Composites 23

2.4.2.1 Imidazole (Anionic Polymerizing) 31

2.7.2.6 Vacuum Bag Molding (Wet Bagging) 47

3 Micro- and Nanoscale Structure Formation in Epoxy-Clay

4 Long Fiber-Reinforced Epoxy Composites 83

5 Eco-Friendly Epoxy-Based Composites 97

5.2 Physical Behavior of Natural Fiber/Filler-Reinforced Epoxy

6 Processing of Epoxy Composites Based on Carbon

7 Thermal Stability and Flame Retardancy of Epoxy

7.2.1.1 Bis(4-cyanato-3,5-dimethylphenyl) Naphthyl Methane/Epoxy/Glass

7.4.3 Epoxy/Glass Fiber (GE) Composites and Epoxy/Glassfiber/Nano Al2 O3

8 Spectroscopy and X-ray Scattering Studies of Epoxy

9 Water Absorption Studies in Epoxy Nanocomposites 241

10 Fracture Surface and Mechanical Properties of Epoxy

10.3.4 Dynamic Mechanical Properties 284

11 Dielectric and Conductivity Studies of Epoxy Composites 299

12 Smart Epoxy Composites 349

13 Projects Using Composite Epoxy Materials: Applications,

Introduction to Epoxy Composites

Epoxy Composites: Fabrication, Characterization and Applications,

epoxy, phosphorus-containing epoxy, and silicon-containing epoxy. While the

1.2 Manufacturing Methods for Fabrication of

1.3 Experimental Techniques for the Characterization of

Table 1.1 Manufacturing techniques used in composite fabrication.

Table 1.1 (Continued)

8. Filament The advantages of filament winding are higher [39, 40]

1.4 Properties of Epoxy Composites

Table 1.2 Characteristic bands of DGEBA.

Band (cm−1 ) FTIR peak assignment

≈3500 O–H stretching

Source: María González et al. [73]. IntechOpen. CC BY 3.0.

(a) (b) (c) (d) (e)

Figure 1.1 Schematic representation of failure types in epoxy/CNT composites: (a)

Untreated CF CF/Ag CF/Ag/GO

Figure 1.3 Schematic representation IFSS increase

1.4.2 Dielectric Properties

1.4.3 Water/Moisture Absorption

30.0 60.0° 30.0 60.0°

thickness of nanosized fillers in epoxy composites. George and Verpoest [113]

In this chapter, an overview of the manufacturing, characterization, and properties

1 Basheer, B.V., George, J.J., Siengchin, S., and Parameswaranpillai, J. (2020).

composites–a comparative study. Composites Science and Technology 65 (15–16):

67 Lupoi, J.S., Singh, S., Parthasarathi, R. et al. (2015). Recent innovations in

Synthesis and Manufacturing of Epoxy Composites